# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dharmaraj Nallasamy' _publ_contact_author_address ; Department of Chemistry Bharathiar University Coimbatore Tamilnadu India 641046 ; _publ_contact_author_email dharmaraj@buc.edu.in loop_ _publ_author_name K.Paramasivam S.Palanisamy R.Butorac A.Cowley N.Bhuvanesh ; D.Nallasamy ; # Attachment '- Complex 3.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 796259' #TrackingRef '- Complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H45 Cu Fe N2 O P2' _chemical_formula_sum 'C54 H45 Cu Fe N2 O P2' _chemical_formula_weight 919.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7088(7) _cell_length_b 17.8387(9) _cell_length_c 20.7620(8) _cell_angle_alpha 90.00 _cell_angle_beta 119.129(2) _cell_angle_gamma 90.00 _cell_volume 4435.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17541 _cell_measurement_theta_min 1.5202 _cell_measurement_theta_max 31.1351 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7328 _exptl_absorpt_correction_T_max 0.8742 _exptl_absorpt_process_details ; Abscor. T. Higashi. (2001). Rigaku Corp. Tokyo, Japan ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+ CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68529 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10114 _reflns_number_gt 9199 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_acknowledgements ; The data were collected using instrumentation purchased with funds provided by the National Science Foundation Grant No. 0741973. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+2.3214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10114 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.78772(14) 1.10752(10) 0.20407(10) 0.0189(3) Uani 1 1 d . . . C2 C 0.78598(15) 1.09699(10) 0.13683(10) 0.0222(4) Uani 1 1 d . . . H2 H 0.7626 1.0502 0.1120 0.027 Uiso 1 1 calc R . . C3 C 0.81845(17) 1.15470(11) 0.10582(11) 0.0269(4) Uani 1 1 d . . . H3 H 0.8185 1.1468 0.0606 0.032 Uiso 1 1 calc R . . C4 C 0.85071(16) 1.22384(11) 0.14119(11) 0.0267(4) Uani 1 1 d . . . H4 H 0.8716 1.2634 0.1197 0.032 Uiso 1 1 calc R . . C5 C 0.85234(16) 1.23481(11) 0.20789(11) 0.0265(4) Uani 1 1 d . . . H5 H 0.8748 1.2819 0.2322 0.032 Uiso 1 1 calc R . . C6 C 0.82108(16) 1.17704(10) 0.23940(11) 0.0236(4) Uani 1 1 d . . . H6 H 0.8225 1.1849 0.2851 0.028 Uiso 1 1 calc R . . C7 C 0.75080(14) 1.04558(9) 0.23634(10) 0.0178(3) Uani 1 1 d . . . C8 C 0.82416(15) 0.97515(10) 0.40700(10) 0.0210(4) Uani 1 1 d . . . H8 H 0.8815 1.0107 0.4338 0.025 Uiso 1 1 calc R . . C9 C 0.80354(16) 0.91753(10) 0.44850(10) 0.0227(4) Uani 1 1 d . . . C10 C 0.73930(16) 0.84995(11) 0.42162(11) 0.0251(4) Uani 1 1 d . . . H10 H 0.7009 0.8344 0.3727 0.030 Uiso 1 1 d R . . C11 C 0.74490(19) 0.81082(13) 0.48350(12) 0.0334(5) Uani 1 1 d . . . H11 H 0.7101 0.7655 0.4817 0.040 Uiso 1 1 d R . . C12 C 0.8129(2) 0.85322(13) 0.54841(12) 0.0365(5) Uani 1 1 d . . . H12 H 0.8300 0.8403 0.5962 0.044 Uiso 1 1 d R . . C13 C 0.85025(19) 0.91855(12) 0.52770(11) 0.0303(4) Uani 1 1 d . . . H13 H 0.8966 0.9555 0.5595 0.036 Uiso 1 1 d R . . C14 C 0.96792(18) 0.76438(13) 0.44220(12) 0.0335(5) Uani 1 1 d . . . H14 H 0.9328 0.7546 0.3919 0.040 Uiso 1 1 d R . . C15 C 1.03780(17) 0.82730(12) 0.47857(12) 0.0316(4) Uani 1 1 d . . . H15 H 1.0560 0.8656 0.4559 0.038 Uiso 1 1 d R . . C16 C 1.07490(17) 0.82139(11) 0.55556(11) 0.0295(4) Uani 1 1 d . . . H16 H 1.1214 0.8549 0.5919 0.035 Uiso 1 1 d R . . C17 C 1.02743(18) 0.75448(11) 0.56664(12) 0.0326(5) Uani 1 1 d . . . H17 H 1.0375 0.7368 0.6116 0.039 Uiso 1 1 d R . . C18 C 0.96160(18) 0.71940(12) 0.49649(12) 0.0350(5) Uani 1 1 d . . . H18 H 0.9217 0.6750 0.4880 0.042 Uiso 1 1 d R . . C19 C 0.44252(15) 0.93285(10) 0.30717(10) 0.0206(3) Uani 1 1 d . . . C20 C 0.35115(16) 0.90648(12) 0.31401(11) 0.0275(4) Uani 1 1 d . . . H20 H 0.3077 0.8658 0.2845 0.033 Uiso 1 1 calc R . . C21 C 0.32447(17) 0.94008(14) 0.36413(12) 0.0333(5) Uani 1 1 d . . . H21 H 0.2637 0.9216 0.3693 0.040 Uiso 1 1 calc R . . C22 C 0.3866(2) 1.00056(13) 0.40651(12) 0.0363(5) Uani 1 1 d . . . H22 H 0.3664 1.0247 0.4391 0.044 Uiso 1 1 calc R . . C23 C 0.4781(2) 1.02544(13) 0.40113(12) 0.0356(5) Uani 1 1 d . . . H23 H 0.5214 1.0661 0.4309 0.043 Uiso 1 1 calc R . . C24 C 0.50694(17) 0.99141(11) 0.35257(11) 0.0266(4) Uani 1 1 d . . . H24 H 0.5710 1.0081 0.3502 0.032 Uiso 1 1 calc R . . C25 C 0.36390(15) 0.93263(10) 0.15132(10) 0.0202(3) Uani 1 1 d . . . C26 C 0.25220(16) 0.90923(11) 0.12310(11) 0.0244(4) Uani 1 1 d . . . H26 H 0.2339 0.8728 0.1488 0.029 Uiso 1 1 calc R . . C27 C 0.16864(16) 0.93959(12) 0.05745(11) 0.0281(4) Uani 1 1 d . . . H27 H 0.0934 0.9240 0.0388 0.034 Uiso 1 1 calc R . . C28 C 0.19483(17) 0.99267(11) 0.01914(11) 0.0287(4) Uani 1 1 d . . . H28 H 0.1375 1.0132 -0.0255 0.034 Uiso 1 1 calc R . . C29 C 0.30538(17) 1.01572(11) 0.04636(11) 0.0274(4) Uani 1 1 d . . . H29 H 0.3233 1.0518 0.0200 0.033 Uiso 1 1 calc R . . C30 C 0.38945(16) 0.98593(10) 0.11207(10) 0.0226(4) Uani 1 1 d . . . H30 H 0.4645 1.0018 0.1304 0.027 Uiso 1 1 calc R . . C31 C 0.44654(14) 0.79641(10) 0.23472(10) 0.0195(3) Uani 1 1 d . . . C32 C 0.47399(15) 0.75703(10) 0.29997(11) 0.0217(4) Uani 1 1 d . . . H32 H 0.4999 0.7835 0.3451 0.026 Uiso 1 1 calc R . . C33 C 0.46337(17) 0.67927(10) 0.29882(12) 0.0259(4) Uani 1 1 d . . . H33 H 0.4824 0.6530 0.3432 0.031 Uiso 1 1 calc R . . C34 C 0.42496(17) 0.64007(11) 0.23301(12) 0.0288(4) Uani 1 1 d . . . H34 H 0.4178 0.5871 0.2324 0.035 Uiso 1 1 calc R . . C35 C 0.39713(17) 0.67836(11) 0.16818(12) 0.0278(4) Uani 1 1 d . . . H35 H 0.3706 0.6515 0.1232 0.033 Uiso 1 1 calc R . . C36 C 0.40796(15) 0.75643(10) 0.16858(11) 0.0236(4) Uani 1 1 d . . . H36 H 0.3892 0.7823 0.1240 0.028 Uiso 1 1 calc R . . C37 C 0.76447(14) 0.73358(9) 0.24670(9) 0.0179(3) Uani 1 1 d . . . C38 C 0.85504(14) 0.69688(10) 0.24695(10) 0.0205(4) Uani 1 1 d . . . H38 H 0.8941 0.7201 0.2250 0.025 Uiso 1 1 calc R . . C39 C 0.88797(17) 0.62615(11) 0.27935(11) 0.0263(4) Uani 1 1 d . . . H39 H 0.9493 0.6013 0.2794 0.032 Uiso 1 1 calc R . . C40 C 0.83073(19) 0.59222(11) 0.31150(12) 0.0306(4) Uani 1 1 d . . . H40 H 0.8540 0.5446 0.3344 0.037 Uiso 1 1 calc R . . C41 C 0.73956(18) 0.62782(11) 0.31023(12) 0.0294(4) Uani 1 1 d . . . H41 H 0.6996 0.6039 0.3312 0.035 Uiso 1 1 calc R . . C42 C 0.70685(16) 0.69843(10) 0.27829(11) 0.0236(4) Uani 1 1 d . . . H42 H 0.6450 0.7228 0.2780 0.028 Uiso 1 1 calc R . . C43 C 0.84284(14) 0.86511(10) 0.20711(10) 0.0192(3) Uani 1 1 d . . . C44 C 0.92213(15) 0.89964(10) 0.27220(11) 0.0243(4) Uani 1 1 d . . . H44 H 0.9101 0.9016 0.3135 0.029 Uiso 1 1 calc R . . C45 C 1.01852(16) 0.93117(11) 0.27715(13) 0.0309(4) Uani 1 1 d . . . H45 H 1.0714 0.9548 0.3215 0.037 Uiso 1 1 calc R . . C46 C 1.03714(17) 0.92799(11) 0.21754(13) 0.0307(5) Uani 1 1 d . . . H46 H 1.1031 0.9492 0.2210 0.037 Uiso 1 1 calc R . . C47 C 0.95959(17) 0.89380(11) 0.15267(12) 0.0285(4) Uani 1 1 d . . . H47 H 0.9728 0.8917 0.1118 0.034 Uiso 1 1 calc R . . C48 C 0.86183(15) 0.86229(11) 0.14676(10) 0.0232(4) Uani 1 1 d . . . H48 H 0.8088 0.8392 0.1021 0.028 Uiso 1 1 calc R . . C49 C 0.61987(14) 0.80839(10) 0.10997(10) 0.0190(3) Uani 1 1 d . . . C50 C 0.58818(15) 0.73593(10) 0.08193(10) 0.0219(4) Uani 1 1 d . . . H50 H 0.6226 0.6938 0.1127 0.026 Uiso 1 1 calc R . . C51 C 0.50549(16) 0.72548(11) 0.00832(11) 0.0254(4) Uani 1 1 d . . . H51 H 0.4838 0.6762 -0.0106 0.030 Uiso 1 1 calc R . . C52 C 0.45523(15) 0.78687(12) -0.03690(10) 0.0252(4) Uani 1 1 d . . . H52 H 0.3988 0.7796 -0.0866 0.030 Uiso 1 1 calc R . . C53 C 0.48773(16) 0.85932(11) -0.00933(11) 0.0267(4) Uani 1 1 d . . . H53 H 0.4543 0.9013 -0.0406 0.032 Uiso 1 1 calc R . . C54 C 0.56914(15) 0.87031(11) 0.06397(10) 0.0231(4) Uani 1 1 d . . . H54 H 0.5902 0.9197 0.0827 0.028 Uiso 1 1 calc R . . Cu1 Cu 0.648273(17) 0.917486(11) 0.253305(11) 0.01682(7) Uani 1 1 d . . . Fe1 Fe 0.90242(2) 0.824795(15) 0.496316(14) 0.02265(8) Uani 1 1 d . . . N1 N 0.80743(12) 1.04096(8) 0.30935(8) 0.0193(3) Uani 1 1 d . . . N2 N 0.76934(12) 0.98108(8) 0.33588(8) 0.0180(3) Uani 1 1 d . . . O1 O 0.66999(10) 1.00338(7) 0.19148(7) 0.0188(2) Uani 1 1 d . . . P1 P 0.47801(4) 0.89645(2) 0.23829(2) 0.01692(10) Uani 1 1 d . . . P2 P 0.71856(4) 0.82733(2) 0.20742(2) 0.01612(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0142(8) 0.0187(8) 0.0218(9) 0.0007(6) 0.0072(7) -0.0006(6) C2 0.0214(9) 0.0222(8) 0.0242(9) -0.0016(7) 0.0119(8) -0.0006(7) C3 0.0276(10) 0.0302(10) 0.0270(10) 0.0029(8) 0.0167(8) 0.0009(8) C4 0.0217(9) 0.0257(9) 0.0341(11) 0.0071(8) 0.0148(8) -0.0015(7) C5 0.0240(9) 0.0206(9) 0.0316(10) -0.0011(7) 0.0110(8) -0.0065(7) C6 0.0246(9) 0.0219(9) 0.0229(9) -0.0019(7) 0.0104(8) -0.0051(7) C7 0.0165(8) 0.0167(8) 0.0204(8) -0.0010(6) 0.0091(7) 0.0000(6) C8 0.0218(9) 0.0195(8) 0.0200(9) -0.0010(6) 0.0088(7) 0.0001(7) C9 0.0243(9) 0.0229(9) 0.0211(9) 0.0017(7) 0.0111(8) 0.0032(7) C10 0.0221(9) 0.0271(9) 0.0257(10) 0.0046(7) 0.0113(8) 0.0007(7) C11 0.0332(11) 0.0353(11) 0.0367(12) 0.0102(9) 0.0209(10) 0.0013(9) C12 0.0475(13) 0.0427(12) 0.0286(11) 0.0068(9) 0.0260(10) 0.0075(10) C13 0.0406(12) 0.0309(10) 0.0215(10) 0.0024(7) 0.0168(9) 0.0084(8) C14 0.0259(10) 0.0415(12) 0.0254(10) -0.0098(9) 0.0066(9) 0.0081(9) C15 0.0237(10) 0.0387(11) 0.0289(11) -0.0007(8) 0.0100(9) 0.0047(8) C16 0.0238(10) 0.0286(10) 0.0243(10) -0.0017(7) 0.0024(8) 0.0014(7) C17 0.0314(11) 0.0236(9) 0.0249(10) 0.0018(8) -0.0004(9) 0.0021(8) C18 0.0299(11) 0.0244(10) 0.0328(11) -0.0047(8) 0.0012(9) 0.0042(8) C19 0.0185(8) 0.0221(8) 0.0202(9) 0.0023(7) 0.0087(7) 0.0049(7) C20 0.0173(9) 0.0387(11) 0.0264(10) -0.0026(8) 0.0105(8) 0.0012(7) C21 0.0208(10) 0.0530(13) 0.0284(10) 0.0012(9) 0.0137(8) 0.0075(9) C22 0.0394(12) 0.0458(13) 0.0275(11) -0.0016(9) 0.0194(10) 0.0142(10) C23 0.0480(13) 0.0312(11) 0.0310(11) -0.0064(9) 0.0218(10) -0.0002(9) C24 0.0320(10) 0.0236(9) 0.0266(10) -0.0010(7) 0.0161(8) 0.0007(8) C25 0.0199(9) 0.0191(8) 0.0208(9) -0.0014(6) 0.0093(7) 0.0009(6) C26 0.0196(9) 0.0267(9) 0.0260(10) 0.0000(7) 0.0105(8) -0.0006(7) C27 0.0203(9) 0.0325(10) 0.0265(10) -0.0013(8) 0.0076(8) 0.0013(8) C28 0.0262(10) 0.0312(10) 0.0225(9) 0.0029(8) 0.0070(8) 0.0072(8) C29 0.0321(10) 0.0251(9) 0.0251(10) 0.0045(7) 0.0141(8) 0.0039(8) C30 0.0225(9) 0.0219(8) 0.0238(9) -0.0013(7) 0.0116(8) 0.0000(7) C31 0.0155(8) 0.0186(8) 0.0258(9) -0.0012(7) 0.0112(7) -0.0008(6) C32 0.0211(9) 0.0209(8) 0.0276(9) 0.0004(7) 0.0154(8) -0.0002(7) C33 0.0275(10) 0.0221(9) 0.0358(11) 0.0037(7) 0.0213(9) 0.0007(7) C34 0.0291(10) 0.0193(9) 0.0466(12) -0.0031(8) 0.0251(10) -0.0039(7) C35 0.0272(10) 0.0233(9) 0.0347(11) -0.0082(8) 0.0164(9) -0.0036(7) C36 0.0216(9) 0.0238(9) 0.0258(9) -0.0022(7) 0.0119(8) -0.0009(7) C37 0.0169(8) 0.0174(8) 0.0178(8) -0.0017(6) 0.0073(7) -0.0009(6) C38 0.0195(9) 0.0209(8) 0.0217(9) -0.0019(7) 0.0104(7) 0.0000(6) C39 0.0253(9) 0.0227(9) 0.0311(10) -0.0008(7) 0.0139(8) 0.0044(7) C40 0.0377(11) 0.0197(9) 0.0358(11) 0.0046(8) 0.0190(10) 0.0046(8) C41 0.0366(11) 0.0220(9) 0.0377(11) 0.0035(8) 0.0244(10) -0.0011(8) C42 0.0237(9) 0.0220(9) 0.0285(10) 0.0005(7) 0.0154(8) 0.0001(7) C43 0.0162(8) 0.0165(8) 0.0240(9) 0.0015(6) 0.0089(7) 0.0016(6) C44 0.0181(9) 0.0254(9) 0.0289(10) -0.0044(7) 0.0112(8) 0.0003(7) C45 0.0177(9) 0.0248(9) 0.0466(13) -0.0075(8) 0.0129(9) -0.0018(7) C46 0.0211(9) 0.0204(9) 0.0526(13) 0.0077(8) 0.0194(9) 0.0026(7) C47 0.0251(10) 0.0299(10) 0.0372(11) 0.0147(8) 0.0204(9) 0.0091(8) C48 0.0203(9) 0.0263(9) 0.0235(9) 0.0056(7) 0.0112(8) 0.0043(7) C49 0.0144(8) 0.0236(8) 0.0190(8) -0.0013(7) 0.0081(7) -0.0010(6) C50 0.0212(9) 0.0225(9) 0.0216(9) -0.0018(7) 0.0101(7) -0.0025(7) C51 0.0227(9) 0.0287(9) 0.0243(9) -0.0062(7) 0.0112(8) -0.0076(7) C52 0.0174(9) 0.0366(10) 0.0182(9) -0.0038(7) 0.0061(7) -0.0033(7) C53 0.0220(9) 0.0304(10) 0.0230(9) 0.0024(7) 0.0073(8) 0.0023(7) C54 0.0213(9) 0.0227(9) 0.0231(9) -0.0007(7) 0.0091(8) 0.0003(7) Cu1 0.01511(12) 0.01628(11) 0.01910(12) -0.00085(7) 0.00836(9) -0.00126(7) Fe1 0.02501(15) 0.02170(14) 0.01760(14) 0.00097(9) 0.00753(12) 0.00139(10) N1 0.0189(7) 0.0167(7) 0.0217(7) 0.0003(5) 0.0094(6) -0.0027(5) N2 0.0168(7) 0.0161(7) 0.0213(7) -0.0003(5) 0.0095(6) -0.0005(5) O1 0.0175(6) 0.0182(6) 0.0194(6) -0.0011(5) 0.0080(5) -0.0036(5) P1 0.0148(2) 0.0167(2) 0.0192(2) -0.00041(16) 0.00827(18) -0.00030(15) P2 0.0140(2) 0.0169(2) 0.0172(2) -0.00093(15) 0.00744(17) -0.00042(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.397(3) . ? C1 C6 1.399(2) . ? C1 C7 1.502(2) . ? C2 C3 1.397(3) . ? C2 H2 0.9500 . ? C3 C4 1.393(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.287(2) . ? C7 N1 1.327(2) . ? C8 N2 1.295(2) . ? C8 C9 1.455(3) . ? C8 H8 0.9500 . ? C9 C10 1.436(3) . ? C9 C13 1.445(3) . ? C9 Fe1 2.0613(18) . ? C10 C11 1.431(3) . ? C10 Fe1 2.0569(19) . ? C10 H10 0.9301 . ? C11 C12 1.426(3) . ? C11 Fe1 2.058(2) . ? C11 H11 0.9303 . ? C12 C13 1.421(3) . ? C12 Fe1 2.055(2) . ? C12 H12 0.9306 . ? C13 Fe1 2.046(2) . ? C13 H13 0.9304 . ? C14 C18 1.420(3) . ? C14 C15 1.429(3) . ? C14 Fe1 2.052(2) . ? C14 H14 0.9293 . ? C15 C16 1.426(3) . ? C15 Fe1 2.061(2) . ? C15 H15 0.9300 . ? C16 C17 1.431(3) . ? C16 Fe1 2.068(2) . ? C16 H16 0.9298 . ? C17 C18 1.431(3) . ? C17 Fe1 2.051(2) . ? C17 H17 0.9297 . ? C18 Fe1 2.047(2) . ? C18 H18 0.9291 . ? C19 C24 1.396(3) . ? C19 C20 1.408(3) . ? C19 P1 1.8389(19) . ? C20 C21 1.395(3) . ? C20 H20 0.9500 . ? C21 C22 1.391(3) . ? C21 H21 0.9500 . ? C22 C23 1.385(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.403(3) . ? C25 C26 1.410(3) . ? C25 P1 1.8369(18) . ? C26 C27 1.394(3) . ? C26 H26 0.9500 . ? C27 C28 1.391(3) . ? C27 H27 0.9500 . ? C28 C29 1.397(3) . ? C28 H28 0.9500 . ? C29 C30 1.393(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.402(3) . ? C31 C32 1.405(3) . ? C31 P1 1.8290(18) . ? C32 C33 1.394(3) . ? C32 H32 0.9500 . ? C33 C34 1.390(3) . ? C33 H33 0.9500 . ? C34 C35 1.387(3) . ? C34 H34 0.9500 . ? C35 C36 1.400(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.397(2) . ? C37 C38 1.402(2) . ? C37 P2 1.8325(18) . ? C38 C39 1.397(3) . ? C38 H38 0.9500 . ? C39 C40 1.392(3) . ? C39 H39 0.9500 . ? C40 C41 1.391(3) . ? C40 H40 0.9500 . ? C41 C42 1.392(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.399(3) . ? C43 C48 1.399(3) . ? C43 P2 1.8352(18) . ? C44 C45 1.393(3) . ? C44 H44 0.9500 . ? C45 C46 1.381(3) . ? C45 H45 0.9500 . ? C46 C47 1.387(3) . ? C46 H46 0.9500 . ? C47 C48 1.403(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.397(2) . ? C49 C54 1.403(3) . ? C49 P2 1.8366(18) . ? C50 C51 1.403(3) . ? C50 H50 0.9500 . ? C51 C52 1.388(3) . ? C51 H51 0.9500 . ? C52 C53 1.396(3) . ? C52 H52 0.9500 . ? C53 C54 1.395(3) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? Cu1 N2 2.0519(15) . ? Cu1 O1 2.1109(12) . ? Cu1 P1 2.2310(5) . ? Cu1 P2 2.3057(5) . ? N1 N2 1.413(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.02(17) . . ? C2 C1 C7 120.08(16) . . ? C6 C1 C7 120.87(16) . . ? C3 C2 C1 120.47(17) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.02(18) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 119.85(18) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.28(18) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.35(18) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? O1 C7 N1 127.52(16) . . ? O1 C7 C1 117.75(15) . . ? N1 C7 C1 114.74(15) . . ? N2 C8 C9 124.12(17) . . ? N2 C8 H8 117.9 . . ? C9 C8 H8 117.9 . . ? C10 C9 C13 107.52(17) . . ? C10 C9 C8 128.48(17) . . ? C13 C9 C8 123.96(18) . . ? C10 C9 Fe1 69.43(10) . . ? C13 C9 Fe1 68.84(11) . . ? C8 C9 Fe1 125.49(13) . . ? C11 C10 C9 107.81(18) . . ? C11 C10 Fe1 69.70(12) . . ? C9 C10 Fe1 69.76(11) . . ? C11 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Fe1 C10 H10 126.0 . . ? C12 C11 C10 108.32(19) . . ? C12 C11 Fe1 69.60(13) . . ? C10 C11 Fe1 69.60(11) . . ? C12 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Fe1 C11 H11 126.6 . . ? C13 C12 C11 108.36(18) . . ? C13 C12 Fe1 69.38(12) . . ? C11 C12 Fe1 69.83(12) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Fe1 C12 H12 126.5 . . ? C12 C13 C9 107.97(19) . . ? C12 C13 Fe1 70.07(12) . . ? C9 C13 Fe1 69.96(11) . . ? C12 C13 H13 126.0 . . ? C9 C13 H13 126.0 . . ? Fe1 C13 H13 125.5 . . ? C18 C14 C15 107.97(19) . . ? C18 C14 Fe1 69.53(12) . . ? C15 C14 Fe1 69.99(12) . . ? C18 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Fe1 C14 H14 126.0 . . ? C16 C15 C14 108.4(2) . . ? C16 C15 Fe1 70.05(13) . . ? C14 C15 Fe1 69.34(12) . . ? C16 C15 H15 125.8 . . ? C14 C15 H15 125.8 . . ? Fe1 C15 H15 126.4 . . ? C15 C16 C17 107.45(18) . . ? C15 C16 Fe1 69.54(12) . . ? C17 C16 Fe1 69.04(12) . . ? C15 C16 H16 126.3 . . ? C17 C16 H16 126.3 . . ? Fe1 C16 H16 126.7 . . ? C16 C17 C18 108.2(2) . . ? C16 C17 Fe1 70.32(11) . . ? C18 C17 Fe1 69.42(11) . . ? C16 C17 H17 126.0 . . ? C18 C17 H17 125.8 . . ? Fe1 C17 H17 125.9 . . ? C14 C18 C17 107.99(19) . . ? C14 C18 Fe1 69.93(12) . . ? C17 C18 Fe1 69.71(12) . . ? C14 C18 H18 126.1 . . ? C17 C18 H18 126.0 . . ? Fe1 C18 H18 125.9 . . ? C24 C19 C20 118.89(18) . . ? C24 C19 P1 118.00(14) . . ? C20 C19 P1 123.06(15) . . ? C21 C20 C19 120.05(19) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.84(19) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.5(2) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 120.46(19) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C30 C25 C26 119.13(17) . . ? C30 C25 P1 118.36(14) . . ? C26 C25 P1 122.51(14) . . ? C27 C26 C25 120.03(18) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.36(18) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.00(18) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.08(18) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.39(18) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C36 C31 C32 119.09(16) . . ? C36 C31 P1 120.32(14) . . ? C32 C31 P1 120.11(14) . . ? C33 C32 C31 120.29(18) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.26(18) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.98(18) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.38(19) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 119.99(18) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C42 C37 C38 119.40(16) . . ? C42 C37 P2 117.93(13) . . ? C38 C37 P2 122.66(14) . . ? C39 C38 C37 120.10(17) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C38 119.87(18) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120.23(18) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.03(18) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C37 120.34(18) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? C44 C43 C48 119.02(17) . . ? C44 C43 P2 116.38(14) . . ? C48 C43 P2 124.59(14) . . ? C45 C44 C43 120.80(19) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C46 C45 C44 120.0(2) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 119.98(18) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 120.63(19) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C43 C48 C47 119.59(18) . . ? C43 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C50 C49 C54 119.60(17) . . ? C50 C49 P2 122.82(14) . . ? C54 C49 P2 117.41(13) . . ? C49 C50 C51 119.95(17) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 120.26(18) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 119.93(18) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 120.24(18) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C49 120.01(17) . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? N2 Cu1 O1 79.09(5) . . ? N2 Cu1 P1 125.13(4) . . ? O1 Cu1 P1 119.00(4) . . ? N2 Cu1 P2 113.59(4) . . ? O1 Cu1 P2 92.52(4) . . ? P1 Cu1 P2 116.364(18) . . ? C13 Fe1 C18 161.77(9) . . ? C13 Fe1 C17 125.01(9) . . ? C18 Fe1 C17 40.87(8) . . ? C13 Fe1 C14 156.55(9) . . ? C18 Fe1 C14 40.54(10) . . ? C17 Fe1 C14 68.40(9) . . ? C13 Fe1 C12 40.54(9) . . ? C18 Fe1 C12 124.28(10) . . ? C17 Fe1 C12 106.40(10) . . ? C14 Fe1 C12 161.80(10) . . ? C13 Fe1 C10 68.99(8) . . ? C18 Fe1 C10 119.09(8) . . ? C17 Fe1 C10 153.54(8) . . ? C14 Fe1 C10 107.85(8) . . ? C12 Fe1 C10 68.57(9) . . ? C13 Fe1 C11 68.46(9) . . ? C18 Fe1 C11 106.20(10) . . ? C17 Fe1 C11 118.59(9) . . ? C14 Fe1 C11 125.22(9) . . ? C12 Fe1 C11 40.58(10) . . ? C10 Fe1 C11 40.70(8) . . ? C13 Fe1 C15 121.60(9) . . ? C18 Fe1 C15 68.26(9) . . ? C17 Fe1 C15 68.12(9) . . ? C14 Fe1 C15 40.67(9) . . ? C12 Fe1 C15 155.35(10) . . ? C10 Fe1 C15 127.12(8) . . ? C11 Fe1 C15 163.51(9) . . ? C13 Fe1 C9 41.20(8) . . ? C18 Fe1 C9 154.83(8) . . ? C17 Fe1 C9 163.61(8) . . ? C14 Fe1 C9 121.20(8) . . ? C12 Fe1 C9 68.56(8) . . ? C10 Fe1 C9 40.81(8) . . ? C11 Fe1 C9 68.43(8) . . ? C15 Fe1 C9 109.56(8) . . ? C13 Fe1 C16 108.08(9) . . ? C18 Fe1 C16 68.56(8) . . ? C17 Fe1 C16 40.65(8) . . ? C14 Fe1 C16 68.40(8) . . ? C12 Fe1 C16 119.79(9) . . ? C10 Fe1 C16 164.49(8) . . ? C11 Fe1 C16 153.79(9) . . ? C15 Fe1 C16 40.41(9) . . ? C9 Fe1 C16 127.12(8) . . ? C7 N1 N2 111.74(14) . . ? C8 N2 N1 112.75(14) . . ? C8 N2 Cu1 133.81(12) . . ? N1 N2 Cu1 113.22(11) . . ? C7 O1 Cu1 108.11(11) . . ? C31 P1 C25 103.41(8) . . ? C31 P1 C19 103.27(8) . . ? C25 P1 C19 102.66(8) . . ? C31 P1 Cu1 112.33(6) . . ? C25 P1 Cu1 114.25(6) . . ? C19 P1 Cu1 119.13(6) . . ? C37 P2 C43 102.61(8) . . ? C37 P2 C49 103.40(8) . . ? C43 P2 C49 104.53(8) . . ? C37 P2 Cu1 125.08(6) . . ? C43 P2 Cu1 108.71(6) . . ? C49 P2 Cu1 110.58(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.8(3) . . . . ? C7 C1 C2 C3 178.96(17) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? C2 C3 C4 C5 1.1(3) . . . . ? C3 C4 C5 C6 -0.4(3) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C2 C1 C6 C5 -0.1(3) . . . . ? C7 C1 C6 C5 -178.27(17) . . . . ? C2 C1 C7 O1 -35.3(2) . . . . ? C6 C1 C7 O1 142.82(17) . . . . ? C2 C1 C7 N1 144.40(17) . . . . ? C6 C1 C7 N1 -37.5(2) . . . . ? N2 C8 C9 C10 13.7(3) . . . . ? N2 C8 C9 C13 -168.53(18) . . . . ? N2 C8 C9 Fe1 104.6(2) . . . . ? C13 C9 C10 C11 1.1(2) . . . . ? C8 C9 C10 C11 179.14(19) . . . . ? Fe1 C9 C10 C11 59.55(14) . . . . ? C13 C9 C10 Fe1 -58.47(14) . . . . ? C8 C9 C10 Fe1 119.6(2) . . . . ? C9 C10 C11 C12 -0.6(2) . . . . ? Fe1 C10 C11 C12 59.00(15) . . . . ? C9 C10 C11 Fe1 -59.59(13) . . . . ? C10 C11 C12 C13 -0.1(3) . . . . ? Fe1 C11 C12 C13 58.86(16) . . . . ? C10 C11 C12 Fe1 -59.00(15) . . . . ? C11 C12 C13 C9 0.8(2) . . . . ? Fe1 C12 C13 C9 59.95(14) . . . . ? C11 C12 C13 Fe1 -59.13(16) . . . . ? C10 C9 C13 C12 -1.2(2) . . . . ? C8 C9 C13 C12 -179.34(18) . . . . ? Fe1 C9 C13 C12 -60.02(15) . . . . ? C10 C9 C13 Fe1 58.84(13) . . . . ? C8 C9 C13 Fe1 -119.32(18) . . . . ? C18 C14 C15 C16 0.0(2) . . . . ? Fe1 C14 C15 C16 59.35(15) . . . . ? C18 C14 C15 Fe1 -59.37(15) . . . . ? C14 C15 C16 C17 -0.1(2) . . . . ? Fe1 C15 C16 C17 58.83(15) . . . . ? C14 C15 C16 Fe1 -58.91(14) . . . . ? C15 C16 C17 C18 0.2(2) . . . . ? Fe1 C16 C17 C18 59.30(15) . . . . ? C15 C16 C17 Fe1 -59.15(15) . . . . ? C15 C14 C18 C17 0.1(2) . . . . ? Fe1 C14 C18 C17 -59.55(15) . . . . ? C15 C14 C18 Fe1 59.67(14) . . . . ? C16 C17 C18 C14 -0.2(3) . . . . ? Fe1 C17 C18 C14 59.69(15) . . . . ? C16 C17 C18 Fe1 -59.86(15) . . . . ? C24 C19 C20 C21 1.7(3) . . . . ? P1 C19 C20 C21 -175.66(16) . . . . ? C19 C20 C21 C22 1.2(3) . . . . ? C20 C21 C22 C23 -2.7(3) . . . . ? C21 C22 C23 C24 1.3(3) . . . . ? C22 C23 C24 C19 1.6(3) . . . . ? C20 C19 C24 C23 -3.1(3) . . . . ? P1 C19 C24 C23 174.40(16) . . . . ? C30 C25 C26 C27 -0.7(3) . . . . ? P1 C25 C26 C27 178.86(15) . . . . ? C25 C26 C27 C28 0.4(3) . . . . ? C26 C27 C28 C29 0.1(3) . . . . ? C27 C28 C29 C30 -0.4(3) . . . . ? C28 C29 C30 C25 0.1(3) . . . . ? C26 C25 C30 C29 0.5(3) . . . . ? P1 C25 C30 C29 -179.12(14) . . . . ? C36 C31 C32 C33 0.3(3) . . . . ? P1 C31 C32 C33 -171.82(14) . . . . ? C31 C32 C33 C34 -0.3(3) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C33 C34 C35 C36 0.3(3) . . . . ? C34 C35 C36 C31 -0.4(3) . . . . ? C32 C31 C36 C35 0.1(3) . . . . ? P1 C31 C36 C35 172.15(15) . . . . ? C42 C37 C38 C39 -0.8(3) . . . . ? P2 C37 C38 C39 178.40(14) . . . . ? C37 C38 C39 C40 -0.1(3) . . . . ? C38 C39 C40 C41 1.2(3) . . . . ? C39 C40 C41 C42 -1.5(3) . . . . ? C40 C41 C42 C37 0.7(3) . . . . ? C38 C37 C42 C41 0.5(3) . . . . ? P2 C37 C42 C41 -178.73(15) . . . . ? C48 C43 C44 C45 0.3(3) . . . . ? P2 C43 C44 C45 -178.95(15) . . . . ? C43 C44 C45 C46 -0.6(3) . . . . ? C44 C45 C46 C47 0.4(3) . . . . ? C45 C46 C47 C48 0.1(3) . . . . ? C44 C43 C48 C47 0.2(3) . . . . ? P2 C43 C48 C47 179.32(14) . . . . ? C46 C47 C48 C43 -0.3(3) . . . . ? C54 C49 C50 C51 -0.5(3) . . . . ? P2 C49 C50 C51 174.71(14) . . . . ? C49 C50 C51 C52 0.2(3) . . . . ? C50 C51 C52 C53 0.6(3) . . . . ? C51 C52 C53 C54 -1.2(3) . . . . ? C52 C53 C54 C49 1.0(3) . . . . ? C50 C49 C54 C53 -0.1(3) . . . . ? P2 C49 C54 C53 -175.55(14) . . . . ? C12 C13 Fe1 C18 -38.8(3) . . . . ? C9 C13 Fe1 C18 -157.5(3) . . . . ? C12 C13 Fe1 C17 -73.22(17) . . . . ? C9 C13 Fe1 C17 167.99(12) . . . . ? C12 C13 Fe1 C14 167.8(2) . . . . ? C9 C13 Fe1 C14 49.0(3) . . . . ? C9 C13 Fe1 C12 -118.79(19) . . . . ? C12 C13 Fe1 C10 81.18(14) . . . . ? C9 C13 Fe1 C10 -37.60(12) . . . . ? C12 C13 Fe1 C11 37.36(13) . . . . ? C9 C13 Fe1 C11 -81.42(13) . . . . ? C12 C13 Fe1 C15 -157.29(13) . . . . ? C9 C13 Fe1 C15 83.92(14) . . . . ? C12 C13 Fe1 C9 118.79(19) . . . . ? C12 C13 Fe1 C16 -114.99(14) . . . . ? C9 C13 Fe1 C16 126.22(13) . . . . ? C14 C18 Fe1 C13 -164.1(3) . . . . ? C17 C18 Fe1 C13 -45.1(4) . . . . ? C14 C18 Fe1 C17 -119.0(2) . . . . ? C17 C18 Fe1 C14 119.0(2) . . . . ? C14 C18 Fe1 C12 166.36(13) . . . . ? C17 C18 Fe1 C12 -74.59(17) . . . . ? C14 C18 Fe1 C10 83.64(14) . . . . ? C17 C18 Fe1 C10 -157.31(13) . . . . ? C14 C18 Fe1 C11 125.75(13) . . . . ? C17 C18 Fe1 C11 -115.20(14) . . . . ? C14 C18 Fe1 C15 -37.80(12) . . . . ? C17 C18 Fe1 C15 81.24(15) . . . . ? C14 C18 Fe1 C9 52.1(3) . . . . ? C17 C18 Fe1 C9 171.18(18) . . . . ? C14 C18 Fe1 C16 -81.41(14) . . . . ? C17 C18 Fe1 C16 37.63(14) . . . . ? C16 C17 Fe1 C13 -76.45(16) . . . . ? C18 C17 Fe1 C13 164.31(14) . . . . ? C16 C17 Fe1 C18 119.2(2) . . . . ? C16 C17 Fe1 C14 81.57(14) . . . . ? C18 C17 Fe1 C14 -37.67(14) . . . . ? C16 C17 Fe1 C12 -116.89(14) . . . . ? C18 C17 Fe1 C12 123.86(15) . . . . ? C16 C17 Fe1 C10 168.39(17) . . . . ? C18 C17 Fe1 C10 49.1(3) . . . . ? C16 C17 Fe1 C11 -159.05(13) . . . . ? C18 C17 Fe1 C11 81.71(17) . . . . ? C16 C17 Fe1 C15 37.64(13) . . . . ? C18 C17 Fe1 C15 -81.61(15) . . . . ? C16 C17 Fe1 C9 -47.4(4) . . . . ? C18 C17 Fe1 C9 -166.6(3) . . . . ? C18 C17 Fe1 C16 -119.2(2) . . . . ? C18 C14 Fe1 C13 167.6(2) . . . . ? C15 C14 Fe1 C13 48.5(3) . . . . ? C15 C14 Fe1 C18 -119.11(18) . . . . ? C18 C14 Fe1 C17 37.97(13) . . . . ? C15 C14 Fe1 C17 -81.14(13) . . . . ? C18 C14 Fe1 C12 -38.6(3) . . . . ? C15 C14 Fe1 C12 -157.7(3) . . . . ? C18 C14 Fe1 C10 -114.16(13) . . . . ? C15 C14 Fe1 C10 126.73(12) . . . . ? C18 C14 Fe1 C11 -72.54(15) . . . . ? C15 C14 Fe1 C11 168.35(12) . . . . ? C18 C14 Fe1 C15 119.11(18) . . . . ? C18 C14 Fe1 C9 -156.89(12) . . . . ? C15 C14 Fe1 C9 84.00(14) . . . . ? C18 C14 Fe1 C16 81.84(13) . . . . ? C15 C14 Fe1 C16 -37.27(12) . . . . ? C11 C12 Fe1 C13 119.79(19) . . . . ? C13 C12 Fe1 C18 166.29(12) . . . . ? C11 C12 Fe1 C18 -73.92(15) . . . . ? C13 C12 Fe1 C17 125.17(13) . . . . ? C11 C12 Fe1 C17 -115.04(13) . . . . ? C13 C12 Fe1 C14 -164.3(3) . . . . ? C11 C12 Fe1 C14 -44.5(3) . . . . ? C13 C12 Fe1 C10 -82.33(14) . . . . ? C11 C12 Fe1 C10 37.46(12) . . . . ? C13 C12 Fe1 C11 -119.79(19) . . . . ? C13 C12 Fe1 C15 52.0(3) . . . . ? C11 C12 Fe1 C15 171.82(19) . . . . ? C13 C12 Fe1 C9 -38.33(13) . . . . ? C11 C12 Fe1 C9 81.46(13) . . . . ? C13 C12 Fe1 C16 83.15(15) . . . . ? C11 C12 Fe1 C16 -157.06(12) . . . . ? C11 C10 Fe1 C13 -80.98(14) . . . . ? C9 C10 Fe1 C13 37.95(11) . . . . ? C11 C10 Fe1 C18 80.95(15) . . . . ? C9 C10 Fe1 C18 -160.11(12) . . . . ? C11 C10 Fe1 C17 46.4(2) . . . . ? C9 C10 Fe1 C17 165.38(18) . . . . ? C11 C10 Fe1 C14 123.69(14) . . . . ? C9 C10 Fe1 C14 -117.38(12) . . . . ? C11 C10 Fe1 C12 -37.35(13) . . . . ? C9 C10 Fe1 C12 81.59(13) . . . . ? C9 C10 Fe1 C11 118.94(17) . . . . ? C11 C10 Fe1 C15 164.61(13) . . . . ? C9 C10 Fe1 C15 -76.45(14) . . . . ? C11 C10 Fe1 C9 -118.94(17) . . . . ? C11 C10 Fe1 C16 -162.9(3) . . . . ? C9 C10 Fe1 C16 -44.0(3) . . . . ? C12 C11 Fe1 C13 -37.33(13) . . . . ? C10 C11 Fe1 C13 82.41(13) . . . . ? C12 C11 Fe1 C18 124.23(13) . . . . ? C10 C11 Fe1 C18 -116.02(13) . . . . ? C12 C11 Fe1 C17 81.83(15) . . . . ? C10 C11 Fe1 C17 -158.42(12) . . . . ? C12 C11 Fe1 C14 164.45(13) . . . . ? C10 C11 Fe1 C14 -75.81(15) . . . . ? C10 C11 Fe1 C12 119.75(18) . . . . ? C12 C11 Fe1 C10 -119.75(18) . . . . ? C12 C11 Fe1 C15 -167.9(3) . . . . ? C10 C11 Fe1 C15 -48.2(4) . . . . ? C12 C11 Fe1 C9 -81.79(13) . . . . ? C10 C11 Fe1 C9 37.95(12) . . . . ? C12 C11 Fe1 C16 50.0(2) . . . . ? C10 C11 Fe1 C16 169.74(17) . . . . ? C16 C15 Fe1 C13 80.76(14) . . . . ? C14 C15 Fe1 C13 -159.52(12) . . . . ? C16 C15 Fe1 C18 -82.03(13) . . . . ? C14 C15 Fe1 C18 37.69(13) . . . . ? C16 C15 Fe1 C17 -37.85(12) . . . . ? C14 C15 Fe1 C17 81.87(13) . . . . ? C16 C15 Fe1 C14 -119.72(18) . . . . ? C16 C15 Fe1 C12 43.8(3) . . . . ? C14 C15 Fe1 C12 163.5(2) . . . . ? C16 C15 Fe1 C10 167.20(12) . . . . ? C14 C15 Fe1 C10 -73.08(15) . . . . ? C16 C15 Fe1 C11 -155.2(3) . . . . ? C14 C15 Fe1 C11 -35.5(4) . . . . ? C16 C15 Fe1 C9 124.80(12) . . . . ? C14 C15 Fe1 C9 -115.48(13) . . . . ? C14 C15 Fe1 C16 119.72(18) . . . . ? C10 C9 Fe1 C13 -119.35(17) . . . . ? C8 C9 Fe1 C13 117.4(2) . . . . ? C10 C9 Fe1 C18 44.3(3) . . . . ? C13 C9 Fe1 C18 163.7(2) . . . . ? C8 C9 Fe1 C18 -78.9(3) . . . . ? C10 C9 Fe1 C17 -156.5(3) . . . . ? C13 C9 Fe1 C17 -37.2(4) . . . . ? C8 C9 Fe1 C17 80.2(4) . . . . ? C10 C9 Fe1 C14 81.20(14) . . . . ? C13 C9 Fe1 C14 -159.45(13) . . . . ? C8 C9 Fe1 C14 -42.08(19) . . . . ? C10 C9 Fe1 C12 -81.61(13) . . . . ? C13 C9 Fe1 C12 37.74(13) . . . . ? C8 C9 Fe1 C12 155.10(19) . . . . ? C13 C9 Fe1 C10 119.35(17) . . . . ? C8 C9 Fe1 C10 -123.3(2) . . . . ? C10 C9 Fe1 C11 -37.85(12) . . . . ? C13 C9 Fe1 C11 81.50(14) . . . . ? C8 C9 Fe1 C11 -161.13(19) . . . . ? C10 C9 Fe1 C15 124.65(12) . . . . ? C13 C9 Fe1 C15 -116.00(13) . . . . ? C8 C9 Fe1 C15 1.37(18) . . . . ? C10 C9 Fe1 C16 166.54(12) . . . . ? C13 C9 Fe1 C16 -74.11(15) . . . . ? C8 C9 Fe1 C16 43.3(2) . . . . ? C15 C16 Fe1 C13 -117.83(13) . . . . ? C17 C16 Fe1 C13 123.11(13) . . . . ? C15 C16 Fe1 C18 81.22(14) . . . . ? C17 C16 Fe1 C18 -37.84(13) . . . . ? C15 C16 Fe1 C17 119.06(18) . . . . ? C15 C16 Fe1 C14 37.50(13) . . . . ? C17 C16 Fe1 C14 -81.56(14) . . . . ? C15 C16 Fe1 C12 -160.58(13) . . . . ? C17 C16 Fe1 C12 80.36(15) . . . . ? C15 C16 Fe1 C10 -41.4(4) . . . . ? C17 C16 Fe1 C10 -160.4(3) . . . . ? C15 C16 Fe1 C11 164.38(19) . . . . ? C17 C16 Fe1 C11 45.3(2) . . . . ? C17 C16 Fe1 C15 -119.06(18) . . . . ? C15 C16 Fe1 C9 -76.03(15) . . . . ? C17 C16 Fe1 C9 164.91(12) . . . . ? O1 C7 N1 N2 0.4(2) . . . . ? C1 C7 N1 N2 -179.28(13) . . . . ? C9 C8 N2 N1 -178.78(16) . . . . ? C9 C8 N2 Cu1 -4.7(3) . . . . ? C7 N1 N2 C8 179.43(15) . . . . ? C7 N1 N2 Cu1 4.06(17) . . . . ? O1 Cu1 N2 C8 -178.85(18) . . . . ? P1 Cu1 N2 C8 63.25(18) . . . . ? P2 Cu1 N2 C8 -90.87(17) . . . . ? O1 Cu1 N2 N1 -4.77(10) . . . . ? P1 Cu1 N2 N1 -122.67(10) . . . . ? P2 Cu1 N2 N1 83.21(11) . . . . ? N1 C7 O1 Cu1 -4.3(2) . . . . ? C1 C7 O1 Cu1 175.31(12) . . . . ? N2 Cu1 O1 C7 4.63(11) . . . . ? P1 Cu1 O1 C7 128.90(10) . . . . ? P2 Cu1 O1 C7 -108.91(11) . . . . ? C36 C31 P1 C25 40.80(16) . . . . ? C32 C31 P1 C25 -147.20(14) . . . . ? C36 C31 P1 C19 147.52(15) . . . . ? C32 C31 P1 C19 -40.48(16) . . . . ? C36 C31 P1 Cu1 -82.87(15) . . . . ? C32 C31 P1 Cu1 89.13(14) . . . . ? C30 C25 P1 C31 -139.22(14) . . . . ? C26 C25 P1 C31 41.20(17) . . . . ? C30 C25 P1 C19 113.60(15) . . . . ? C26 C25 P1 C19 -65.98(17) . . . . ? C30 C25 P1 Cu1 -16.82(16) . . . . ? C26 C25 P1 Cu1 163.60(13) . . . . ? C24 C19 P1 C31 145.57(15) . . . . ? C20 C19 P1 C31 -37.07(18) . . . . ? C24 C19 P1 C25 -107.15(15) . . . . ? C20 C19 P1 C25 70.22(17) . . . . ? C24 C19 P1 Cu1 20.23(17) . . . . ? C20 C19 P1 Cu1 -162.40(14) . . . . ? N2 Cu1 P1 C31 -124.96(8) . . . . ? O1 Cu1 P1 C31 137.84(8) . . . . ? P2 Cu1 P1 C31 28.52(7) . . . . ? N2 Cu1 P1 C25 117.65(8) . . . . ? O1 Cu1 P1 C25 20.45(8) . . . . ? P2 Cu1 P1 C25 -88.87(6) . . . . ? N2 Cu1 P1 C19 -4.10(9) . . . . ? O1 Cu1 P1 C19 -101.30(8) . . . . ? P2 Cu1 P1 C19 149.38(7) . . . . ? C42 C37 P2 C43 158.52(14) . . . . ? C38 C37 P2 C43 -20.67(17) . . . . ? C42 C37 P2 C49 -92.97(15) . . . . ? C38 C37 P2 C49 87.84(16) . . . . ? C42 C37 P2 Cu1 34.55(17) . . . . ? C38 C37 P2 Cu1 -144.64(12) . . . . ? C44 C43 P2 C37 -85.92(15) . . . . ? C48 C43 P2 C37 94.89(16) . . . . ? C44 C43 P2 C49 166.43(14) . . . . ? C48 C43 P2 C49 -12.77(17) . . . . ? C44 C43 P2 Cu1 48.31(15) . . . . ? C48 C43 P2 Cu1 -130.88(14) . . . . ? C50 C49 P2 C37 4.80(17) . . . . ? C54 C49 P2 C37 -179.92(14) . . . . ? C50 C49 P2 C43 111.88(16) . . . . ? C54 C49 P2 C43 -72.84(15) . . . . ? C50 C49 P2 Cu1 -131.30(14) . . . . ? C54 C49 P2 Cu1 43.98(15) . . . . ? N2 Cu1 P2 C37 85.40(8) . . . . ? O1 Cu1 P2 C37 164.59(8) . . . . ? P1 Cu1 P2 C37 -71.12(7) . . . . ? N2 Cu1 P2 C43 -35.91(8) . . . . ? O1 Cu1 P2 C43 43.29(7) . . . . ? P1 Cu1 P2 C43 167.58(6) . . . . ? N2 Cu1 P2 C49 -150.12(8) . . . . ? O1 Cu1 P2 C49 -70.93(7) . . . . ? P1 Cu1 P2 C49 53.36(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.489 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.078 # Attachment '- Complex 5.cif' data_nifff _database_code_depnum_ccdc_archive 'CCDC 822888' #TrackingRef '- Complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H31 Cl3 Fe2 N4 Ni O2' _chemical_formula_weight 840.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.2656(8) _cell_length_b 12.9068(6) _cell_length_c 16.8967(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.378(3) _cell_angle_gamma 90.00 _cell_volume 3385.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9861 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 62.74 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 9.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1092 _exptl_absorpt_correction_T_max 0.5869 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 74123 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 59.99 _reflns_number_total 5006 _reflns_number_gt 4541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+4.9075P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00156(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5006 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.91204(3) 0.17991(4) 0.99286(3) 0.01224(16) Uani 1 1 d . . . Fe1 Fe 0.99307(3) 0.53925(4) 1.19323(3) 0.01217(15) Uani 1 1 d . . . Fe2 Fe 0.81962(3) -0.02634(4) 0.68430(3) 0.01175(15) Uani 1 1 d . . . C1 C 0.7778(2) 0.2435(2) 1.03316(19) 0.0139(7) Uani 1 1 d . . . C2 C 0.6863(2) 0.2553(3) 1.0315(2) 0.0153(7) Uani 1 1 d . . . C3 C 0.6630(2) 0.3236(3) 1.0848(2) 0.0234(8) Uani 1 1 d . . . H3A H 0.7062 0.3632 1.1231 0.028 Uiso 1 1 calc R . . C4 C 0.5777(2) 0.3344(3) 1.0824(2) 0.0317(10) Uani 1 1 d . . . H4A H 0.5624 0.3810 1.1192 0.038 Uiso 1 1 calc R . . C5 C 0.5147(2) 0.2771(3) 1.0263(2) 0.0292(9) Uani 1 1 d . . . H5A H 0.4561 0.2846 1.0246 0.035 Uiso 1 1 calc R . . C6 C 0.5368(2) 0.2091(3) 0.9729(2) 0.0248(9) Uani 1 1 d . . . H6A H 0.4934 0.1700 0.9344 0.030 Uiso 1 1 calc R . . C7 C 0.6225(2) 0.1982(3) 0.9757(2) 0.0185(8) Uani 1 1 d . . . H7A H 0.6376 0.1511 0.9391 0.022 Uiso 1 1 calc R . . C8 C 1.0480(2) 0.1149(2) 0.95742(19) 0.0120(7) Uani 1 1 d . . . C9 C 1.1408(2) 0.1056(2) 0.96406(19) 0.0135(7) Uani 1 1 d . . . C10 C 1.1701(2) 0.0315(3) 0.9186(2) 0.0180(8) Uani 1 1 d . . . H10A H 1.1300 -0.0110 0.8796 0.022 Uiso 1 1 calc R . . C11 C 1.2578(2) 0.0200(3) 0.9304(2) 0.0208(8) Uani 1 1 d . . . H11A H 1.2776 -0.0309 0.8998 0.025 Uiso 1 1 calc R . . C12 C 1.3165(2) 0.0821(3) 0.9863(2) 0.0216(8) Uani 1 1 d . . . H12A H 1.3764 0.0733 0.9946 0.026 Uiso 1 1 calc R . . C13 C 1.2878(2) 0.1571(3) 1.0301(2) 0.0194(8) Uani 1 1 d . . . H13A H 1.3281 0.2010 1.0675 0.023 Uiso 1 1 calc R . . C14 C 1.2005(2) 0.1684(3) 1.0197(2) 0.0165(7) Uani 1 1 d . . . H14A H 1.1813 0.2193 1.0507 0.020 Uiso 1 1 calc R . . C15 C 0.9850(2) 0.3136(2) 1.12936(19) 0.0122(7) Uani 1 1 d . . . H15A H 1.0373 0.2992 1.1172 0.015 Uiso 1 1 calc R . . C16 C 0.9934(2) 0.3808(3) 1.19969(19) 0.0146(7) Uani 1 1 d . . . C17 C 1.0757(2) 0.4222(2) 1.2469(2) 0.0160(7) Uani 1 1 d . . . H17A H 1.1322 0.4072 1.2372 0.019 Uiso 1 1 calc R . . C18 C 1.0629(2) 0.4877(3) 1.3091(2) 0.0172(8) Uani 1 1 d . . . H18A H 1.1087 0.5275 1.3508 0.021 Uiso 1 1 calc R . . C19 C 0.9727(2) 0.4890(3) 1.3010(2) 0.0181(8) Uani 1 1 d . . . H19A H 0.9448 0.5299 1.3362 0.022 Uiso 1 1 calc R . . C20 C 0.9296(2) 0.4243(3) 1.2341(2) 0.0153(7) Uani 1 1 d . . . H20A H 0.8663 0.4107 1.2142 0.018 Uiso 1 1 calc R . . C21 C 0.9603(2) 0.5816(3) 1.0709(2) 0.0181(8) Uani 1 1 d . . . H21A H 0.9458 0.5333 1.0224 0.022 Uiso 1 1 calc R . . C22 C 1.0439(2) 0.6190(3) 1.1140(2) 0.0199(8) Uani 1 1 d . . . H22A H 1.0985 0.6018 1.1012 0.024 Uiso 1 1 calc R . . C23 C 1.0361(2) 0.6851(3) 1.1783(2) 0.0196(8) Uani 1 1 d . . . H23A H 1.0843 0.7227 1.2190 0.023 Uiso 1 1 calc R . . C24 C 0.9477(2) 0.6883(3) 1.1751(2) 0.0215(8) Uani 1 1 d . . . H24A H 0.9231 0.7285 1.2133 0.026 Uiso 1 1 calc R . . C25 C 0.9007(2) 0.6249(3) 1.1088(2) 0.0188(8) Uani 1 1 d . . . H25A H 0.8372 0.6123 1.0918 0.023 Uiso 1 1 calc R . . C26 C 0.8441(2) 0.0302(2) 0.86661(19) 0.0130(7) Uani 1 1 d . . . H26A H 0.7903 0.0487 0.8738 0.016 Uiso 1 1 calc R . . C27 C 0.84116(19) -0.0526(2) 0.80799(19) 0.0130(7) Uani 1 1 d . . . C28 C 0.7616(2) -0.1003(3) 0.7602(2) 0.0152(7) Uani 1 1 d . . . H28A H 0.7030 -0.0845 0.7649 0.018 Uiso 1 1 calc R . . C29 C 0.7804(2) -0.1729(2) 0.7048(2) 0.0165(7) Uani 1 1 d . . . H29A H 0.7376 -0.2168 0.6637 0.020 Uiso 1 1 calc R . . C30 C 0.8715(2) -0.1705(2) 0.71747(19) 0.0158(7) Uani 1 1 d . . . H30A H 0.9032 -0.2126 0.6864 0.019 Uiso 1 1 calc R . . C31 C 0.9088(2) -0.0974(2) 0.7804(2) 0.0146(7) Uani 1 1 d . . . H31A H 0.9714 -0.0794 0.8016 0.018 Uiso 1 1 calc R . . C32 C 0.7701(2) 0.0073(3) 0.5603(2) 0.0226(8) Uani 1 1 d . . . H32A H 0.7376 -0.0415 0.5160 0.027 Uiso 1 1 calc R . . C33 C 0.8608(2) 0.0218(3) 0.5873(2) 0.0245(9) Uani 1 1 d . . . H33A H 0.9034 -0.0149 0.5651 0.029 Uiso 1 1 calc R . . C34 C 0.8806(2) 0.0971(3) 0.6519(2) 0.0228(8) Uani 1 1 d . . . H34A H 0.9394 0.1230 0.6827 0.027 Uiso 1 1 calc R . . C35 C 0.8018(2) 0.1292(3) 0.6644(2) 0.0199(8) Uani 1 1 d . . . H35A H 0.7954 0.1815 0.7059 0.024 Uiso 1 1 calc R . . C36 C 0.7338(2) 0.0739(3) 0.6079(2) 0.0197(8) Uani 1 1 d . . . H36A H 0.6712 0.0800 0.6031 0.024 Uiso 1 1 calc R . . N1 N 0.91696(16) 0.2700(2) 1.08023(16) 0.0129(6) Uani 1 1 d . . . N2 N 0.83665(16) 0.2903(2) 1.09244(16) 0.0153(6) Uani 1 1 d . . . N3 N 0.90983(16) 0.0828(2) 0.91068(16) 0.0131(6) Uani 1 1 d . . . N4 N 0.99177(16) 0.0604(2) 0.90206(16) 0.0131(6) Uani 1 1 d . . . O1 O 0.79441(13) 0.18776(17) 0.97572(13) 0.0146(5) Uani 1 1 d . . . O2 O 1.02864(13) 0.17792(16) 1.00958(13) 0.0141(5) Uani 1 1 d . . . C70 C 0.8154(2) 0.1715(3) 0.2676(2) 0.0299(9) Uani 1 1 d . . . H70A H 0.8027 0.1966 0.2092 0.036 Uiso 1 1 calc R . . Cl71 Cl 0.92174(7) 0.12789(10) 0.30124(7) 0.0499(3) Uani 1 1 d . . . Cl72 Cl 0.79827(7) 0.27369(8) 0.32917(7) 0.0417(3) Uani 1 1 d . . . Cl73 Cl 0.74433(7) 0.06926(9) 0.26977(7) 0.0475(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0116(3) 0.0135(3) 0.0123(3) -0.0019(2) 0.0044(2) -0.0007(2) Fe1 0.0132(3) 0.0114(3) 0.0110(3) 0.0004(2) 0.0022(2) 0.0002(2) Fe2 0.0128(3) 0.0118(3) 0.0109(3) 0.0000(2) 0.0037(2) 0.0008(2) C1 0.0175(18) 0.0132(18) 0.0117(18) 0.0030(14) 0.0055(15) -0.0010(14) C2 0.0156(18) 0.0166(19) 0.0142(18) 0.0002(14) 0.0054(14) 0.0002(14) C3 0.0180(19) 0.029(2) 0.023(2) -0.0094(16) 0.0058(16) -0.0023(15) C4 0.025(2) 0.040(3) 0.034(2) -0.0153(19) 0.0148(18) -0.0005(18) C5 0.0153(19) 0.038(2) 0.036(2) -0.0063(19) 0.0119(17) -0.0020(17) C6 0.018(2) 0.028(2) 0.027(2) -0.0071(17) 0.0048(16) -0.0066(16) C7 0.0199(19) 0.021(2) 0.0172(19) -0.0012(14) 0.0086(15) 0.0014(14) C8 0.0179(17) 0.0070(17) 0.0130(18) 0.0055(13) 0.0074(14) 0.0020(13) C9 0.0165(17) 0.0118(18) 0.0130(18) 0.0053(13) 0.0056(14) 0.0003(13) C10 0.0186(19) 0.019(2) 0.0161(19) -0.0013(14) 0.0053(15) -0.0022(14) C11 0.0225(19) 0.021(2) 0.023(2) 0.0013(15) 0.0136(16) 0.0050(15) C12 0.0137(18) 0.028(2) 0.022(2) 0.0088(16) 0.0051(16) 0.0035(15) C13 0.0156(18) 0.024(2) 0.0167(19) 0.0011(15) 0.0014(15) -0.0034(15) C14 0.0210(19) 0.0148(19) 0.0152(19) 0.0016(14) 0.0076(15) 0.0016(14) C15 0.0148(17) 0.0099(17) 0.0125(18) 0.0019(13) 0.0051(14) 0.0014(13) C16 0.0149(17) 0.0153(18) 0.0121(18) 0.0025(14) 0.0016(14) 0.0004(14) C17 0.0182(18) 0.0136(18) 0.0143(19) 0.0048(14) 0.0018(15) 0.0026(14) C18 0.0209(19) 0.0155(19) 0.0123(19) 0.0041(14) 0.0007(15) -0.0005(14) C19 0.027(2) 0.0172(19) 0.0116(19) 0.0003(14) 0.0088(15) 0.0000(15) C20 0.0199(18) 0.0138(18) 0.0125(18) -0.0003(14) 0.0053(14) -0.0007(14) C21 0.0220(19) 0.019(2) 0.0120(19) 0.0051(14) 0.0031(15) 0.0010(14) C22 0.0206(19) 0.020(2) 0.020(2) 0.0080(15) 0.0078(15) -0.0013(15) C23 0.0191(18) 0.0116(19) 0.024(2) 0.0029(15) 0.0004(15) -0.0015(14) C24 0.028(2) 0.015(2) 0.022(2) 0.0036(15) 0.0070(16) 0.0035(15) C25 0.0194(18) 0.0178(19) 0.018(2) 0.0062(15) 0.0042(15) 0.0034(15) C26 0.0154(17) 0.0139(18) 0.0114(18) 0.0016(13) 0.0068(14) -0.0001(14) C27 0.0158(17) 0.0112(18) 0.0119(18) 0.0029(13) 0.0042(14) -0.0007(13) C28 0.0159(18) 0.0167(19) 0.0136(18) 0.0002(14) 0.0054(14) -0.0011(14) C29 0.0204(18) 0.0131(18) 0.0137(19) -0.0013(14) 0.0013(15) -0.0036(14) C30 0.0191(18) 0.0138(19) 0.0127(18) 0.0015(14) 0.0021(14) 0.0056(14) C31 0.0129(17) 0.0158(19) 0.0135(18) 0.0021(14) 0.0015(14) 0.0055(13) C32 0.033(2) 0.019(2) 0.013(2) 0.0044(15) 0.0023(16) 0.0028(16) C33 0.033(2) 0.023(2) 0.024(2) 0.0064(16) 0.0177(17) 0.0021(16) C34 0.025(2) 0.020(2) 0.025(2) 0.0038(16) 0.0098(16) -0.0048(15) C35 0.030(2) 0.0161(19) 0.0152(19) 0.0036(14) 0.0087(16) 0.0016(15) C36 0.0215(19) 0.019(2) 0.0162(19) 0.0082(15) 0.0021(15) 0.0088(15) N1 0.0131(14) 0.0132(15) 0.0125(15) 0.0018(11) 0.0042(12) 0.0011(11) N2 0.0135(14) 0.0154(16) 0.0176(16) -0.0032(12) 0.0054(12) 0.0003(12) N3 0.0125(14) 0.0164(15) 0.0117(15) 0.0019(12) 0.0058(12) -0.0014(11) N4 0.0119(14) 0.0132(15) 0.0156(16) 0.0000(12) 0.0060(12) 0.0000(11) O1 0.0125(11) 0.0177(13) 0.0148(13) -0.0036(9) 0.0058(10) -0.0020(9) O2 0.0132(12) 0.0159(13) 0.0128(12) -0.0028(9) 0.0035(9) -0.0019(9) C70 0.032(2) 0.034(2) 0.029(2) -0.0036(17) 0.0177(18) -0.0088(18) Cl71 0.0317(6) 0.0618(8) 0.0601(8) -0.0158(6) 0.0196(5) 0.0001(5) Cl72 0.0484(6) 0.0380(6) 0.0505(7) -0.0150(5) 0.0325(5) -0.0077(5) Cl73 0.0522(7) 0.0506(7) 0.0504(7) -0.0185(5) 0.0315(6) -0.0291(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.832(2) . ? Ni1 O1 1.850(2) . ? Ni1 N1 1.862(3) . ? Ni1 N3 1.863(3) . ? Fe1 C20 2.042(3) . ? Fe1 C17 2.045(3) . ? Fe1 C22 2.048(3) . ? Fe1 C16 2.048(3) . ? Fe1 C21 2.049(3) . ? Fe1 C23 2.049(3) . ? Fe1 C24 2.051(3) . ? Fe1 C19 2.052(3) . ? Fe1 C25 2.057(3) . ? Fe1 C18 2.059(3) . ? Fe2 C34 2.036(3) . ? Fe2 C27 2.042(3) . ? Fe2 C35 2.042(3) . ? Fe2 C28 2.043(3) . ? Fe2 C31 2.043(3) . ? Fe2 C33 2.043(3) . ? Fe2 C30 2.051(3) . ? Fe2 C36 2.053(3) . ? Fe2 C32 2.054(3) . ? Fe2 C29 2.059(3) . ? C1 O1 1.300(4) . ? C1 N2 1.308(4) . ? C1 C2 1.488(4) . ? C2 C7 1.388(5) . ? C2 C3 1.391(5) . ? C3 C4 1.384(5) . ? C3 H3A 0.9500 . ? C4 C5 1.383(5) . ? C4 H4A 0.9500 . ? C5 C6 1.381(5) . ? C5 H5A 0.9500 . ? C6 C7 1.388(5) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 N4 1.302(4) . ? C8 O2 1.305(4) . ? C8 C9 1.485(4) . ? C9 C14 1.392(5) . ? C9 C10 1.397(5) . ? C10 C11 1.388(5) . ? C10 H10A 0.9500 . ? C11 C12 1.381(5) . ? C11 H11A 0.9500 . ? C12 C13 1.381(5) . ? C12 H12A 0.9500 . ? C13 C14 1.386(5) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 N1 1.298(4) . ? C15 C16 1.444(4) . ? C15 H15A 0.9500 . ? C16 C17 1.441(5) . ? C16 C20 1.445(4) . ? C17 C18 1.412(5) . ? C17 H17A 1.0000 . ? C18 C19 1.432(5) . ? C18 H18A 1.0000 . ? C19 C20 1.413(5) . ? C19 H19A 1.0000 . ? C20 H20A 1.0000 . ? C21 C22 1.422(5) . ? C21 C25 1.426(5) . ? C21 H21A 1.0000 . ? C22 C23 1.417(5) . ? C22 H22A 1.0000 . ? C23 C24 1.423(5) . ? C23 H23A 1.0000 . ? C24 C25 1.413(5) . ? C24 H24A 1.0000 . ? C25 H25A 1.0000 . ? C26 N3 1.297(4) . ? C26 C27 1.448(4) . ? C26 H26A 0.9500 . ? C27 C31 1.439(4) . ? C27 C28 1.443(4) . ? C28 C29 1.420(5) . ? C28 H28A 1.0000 . ? C29 C30 1.433(5) . ? C29 H29A 1.0000 . ? C30 C31 1.416(5) . ? C30 H30A 1.0000 . ? C31 H31A 1.0000 . ? C32 C36 1.421(5) . ? C32 C33 1.421(5) . ? C32 H32A 1.0000 . ? C33 C34 1.425(5) . ? C33 H33A 1.0000 . ? C34 C35 1.422(5) . ? C34 H34A 1.0000 . ? C35 C36 1.419(5) . ? C35 H35A 1.0000 . ? C36 H36A 1.0000 . ? N1 N2 1.407(4) . ? N3 N4 1.413(4) . ? C70 Cl71 1.745(4) . ? C70 Cl72 1.753(4) . ? C70 Cl73 1.762(4) . ? C70 H70A 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O1 177.66(10) . . ? O2 Ni1 N1 95.11(10) . . ? O1 Ni1 N1 83.54(10) . . ? O2 Ni1 N3 83.93(10) . . ? O1 Ni1 N3 97.54(10) . . ? N1 Ni1 N3 176.16(12) . . ? C20 Fe1 C17 69.18(13) . . ? C20 Fe1 C22 158.37(14) . . ? C17 Fe1 C22 108.72(13) . . ? C20 Fe1 C16 41.39(12) . . ? C17 Fe1 C16 41.21(13) . . ? C22 Fe1 C16 122.78(13) . . ? C20 Fe1 C21 121.99(14) . . ? C17 Fe1 C21 125.66(13) . . ? C22 Fe1 C21 40.60(13) . . ? C16 Fe1 C21 108.42(13) . . ? C20 Fe1 C23 159.14(13) . . ? C17 Fe1 C23 122.00(13) . . ? C22 Fe1 C23 40.46(14) . . ? C16 Fe1 C23 158.14(13) . . ? C21 Fe1 C23 68.06(14) . . ? C20 Fe1 C24 122.45(13) . . ? C17 Fe1 C24 156.75(14) . . ? C22 Fe1 C24 68.21(14) . . ? C16 Fe1 C24 160.04(13) . . ? C21 Fe1 C24 68.01(14) . . ? C23 Fe1 C24 40.61(14) . . ? C20 Fe1 C19 40.37(13) . . ? C17 Fe1 C19 68.40(13) . . ? C22 Fe1 C19 160.52(14) . . ? C16 Fe1 C19 68.64(13) . . ? C21 Fe1 C19 156.61(14) . . ? C23 Fe1 C19 123.42(14) . . ? C24 Fe1 C19 106.40(14) . . ? C20 Fe1 C25 106.67(14) . . ? C17 Fe1 C25 162.05(14) . . ? C22 Fe1 C25 68.33(13) . . ? C16 Fe1 C25 124.28(13) . . ? C21 Fe1 C25 40.64(13) . . ? C23 Fe1 C25 68.07(14) . . ? C24 Fe1 C25 40.25(14) . . ? C19 Fe1 C25 120.48(13) . . ? C20 Fe1 C18 68.56(13) . . ? C17 Fe1 C18 40.25(13) . . ? C22 Fe1 C18 124.62(14) . . ? C16 Fe1 C18 68.58(13) . . ? C21 Fe1 C18 161.66(13) . . ? C23 Fe1 C18 107.58(14) . . ? C24 Fe1 C18 121.11(14) . . ? C19 Fe1 C18 40.79(13) . . ? C25 Fe1 C18 156.08(13) . . ? C34 Fe2 C27 117.18(14) . . ? C34 Fe2 C35 40.83(14) . . ? C27 Fe2 C35 107.69(13) . . ? C34 Fe2 C28 152.66(14) . . ? C27 Fe2 C28 41.39(13) . . ? C35 Fe2 C28 119.54(13) . . ? C34 Fe2 C31 106.12(14) . . ? C27 Fe2 C31 41.25(12) . . ? C35 Fe2 C31 127.18(14) . . ? C28 Fe2 C31 69.08(13) . . ? C34 Fe2 C33 40.88(14) . . ? C27 Fe2 C33 150.97(14) . . ? C35 Fe2 C33 68.54(14) . . ? C28 Fe2 C33 165.79(14) . . ? C31 Fe2 C33 116.66(14) . . ? C34 Fe2 C30 126.14(14) . . ? C27 Fe2 C30 68.84(13) . . ? C35 Fe2 C30 164.53(14) . . ? C28 Fe2 C30 68.53(13) . . ? C31 Fe2 C30 40.46(13) . . ? C33 Fe2 C30 106.75(14) . . ? C34 Fe2 C36 68.42(14) . . ? C27 Fe2 C36 128.65(13) . . ? C35 Fe2 C36 40.54(14) . . ? C28 Fe2 C36 109.52(13) . . ? C31 Fe2 C36 166.11(14) . . ? C33 Fe2 C36 68.20(14) . . ? C30 Fe2 C36 152.99(14) . . ? C34 Fe2 C32 68.55(15) . . ? C27 Fe2 C32 166.98(13) . . ? C35 Fe2 C32 68.35(14) . . ? C28 Fe2 C32 128.70(14) . . ? C31 Fe2 C32 151.00(13) . . ? C33 Fe2 C32 40.57(15) . . ? C30 Fe2 C32 118.34(14) . . ? C36 Fe2 C32 40.49(14) . . ? C34 Fe2 C29 164.73(14) . . ? C27 Fe2 C29 69.03(13) . . ? C35 Fe2 C29 153.51(13) . . ? C28 Fe2 C29 40.53(13) . . ? C31 Fe2 C29 68.66(13) . . ? C33 Fe2 C29 127.35(14) . . ? C30 Fe2 C29 40.82(13) . . ? C36 Fe2 C29 119.88(14) . . ? C32 Fe2 C29 108.62(14) . . ? O1 C1 N2 124.1(3) . . ? O1 C1 C2 118.2(3) . . ? N2 C1 C2 117.8(3) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 C1 120.0(3) . . ? C3 C2 C1 121.1(3) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C6 C5 C4 120.2(3) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C7 119.8(3) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C6 C7 C2 120.6(3) . . ? C6 C7 H7A 119.7 . . ? C2 C7 H7A 119.7 . . ? N4 C8 O2 124.3(3) . . ? N4 C8 C9 119.4(3) . . ? O2 C8 C9 116.3(3) . . ? C14 C9 C10 119.1(3) . . ? C14 C9 C8 119.5(3) . . ? C10 C9 C8 121.3(3) . . ? C11 C10 C9 119.9(3) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C13 C14 C9 120.4(3) . . ? C13 C14 H14A 119.8 . . ? C9 C14 H14A 119.8 . . ? N1 C15 C16 129.8(3) . . ? N1 C15 H15A 115.1 . . ? C16 C15 H15A 115.1 . . ? C17 C16 C15 121.5(3) . . ? C17 C16 C20 107.0(3) . . ? C15 C16 C20 131.4(3) . . ? C17 C16 Fe1 69.29(19) . . ? C15 C16 Fe1 123.9(2) . . ? C20 C16 Fe1 69.08(19) . . ? C18 C17 C16 108.4(3) . . ? C18 C17 Fe1 70.37(19) . . ? C16 C17 Fe1 69.50(18) . . ? C18 C17 H17A 125.8 . . ? C16 C17 H17A 125.8 . . ? Fe1 C17 H17A 125.8 . . ? C17 C18 C19 108.1(3) . . ? C17 C18 Fe1 69.37(18) . . ? C19 C18 Fe1 69.34(18) . . ? C17 C18 H18A 125.9 . . ? C19 C18 H18A 125.9 . . ? Fe1 C18 H18A 125.9 . . ? C20 C19 C18 108.5(3) . . ? C20 C19 Fe1 69.45(18) . . ? C18 C19 Fe1 69.87(18) . . ? C20 C19 H19A 125.7 . . ? C18 C19 H19A 125.7 . . ? Fe1 C19 H19A 125.7 . . ? C19 C20 C16 108.0(3) . . ? C19 C20 Fe1 70.18(19) . . ? C16 C20 Fe1 69.54(18) . . ? C19 C20 H20A 126.0 . . ? C16 C20 H20A 126.0 . . ? Fe1 C20 H20A 126.0 . . ? C22 C21 C25 108.1(3) . . ? C22 C21 Fe1 69.65(19) . . ? C25 C21 Fe1 69.98(19) . . ? C22 C21 H21A 125.9 . . ? C25 C21 H21A 125.9 . . ? Fe1 C21 H21A 125.9 . . ? C23 C22 C21 107.8(3) . . ? C23 C22 Fe1 69.83(19) . . ? C21 C22 Fe1 69.74(18) . . ? C23 C22 H22A 126.1 . . ? C21 C22 H22A 126.1 . . ? Fe1 C22 H22A 126.1 . . ? C22 C23 C24 108.1(3) . . ? C22 C23 Fe1 69.71(19) . . ? C24 C23 Fe1 69.76(19) . . ? C22 C23 H23A 126.0 . . ? C24 C23 H23A 126.0 . . ? Fe1 C23 H23A 126.0 . . ? C25 C24 C23 108.3(3) . . ? C25 C24 Fe1 70.10(19) . . ? C23 C24 Fe1 69.63(19) . . ? C25 C24 H24A 125.9 . . ? C23 C24 H24A 125.9 . . ? Fe1 C24 H24A 125.9 . . ? C24 C25 C21 107.7(3) . . ? C24 C25 Fe1 69.65(19) . . ? C21 C25 Fe1 69.38(19) . . ? C24 C25 H25A 126.1 . . ? C21 C25 H25A 126.1 . . ? Fe1 C25 H25A 126.1 . . ? N3 C26 C27 129.2(3) . . ? N3 C26 H26A 115.4 . . ? C27 C26 H26A 115.4 . . ? C31 C27 C28 107.0(3) . . ? C31 C27 C26 130.2(3) . . ? C28 C27 C26 122.6(3) . . ? C31 C27 Fe2 69.44(18) . . ? C28 C27 Fe2 69.35(18) . . ? C26 C27 Fe2 122.6(2) . . ? C29 C28 C27 108.4(3) . . ? C29 C28 Fe2 70.34(18) . . ? C27 C28 Fe2 69.27(17) . . ? C29 C28 H28A 125.8 . . ? C27 C28 H28A 125.8 . . ? Fe2 C28 H28A 125.8 . . ? C28 C29 C30 107.7(3) . . ? C28 C29 Fe2 69.13(18) . . ? C30 C29 Fe2 69.30(18) . . ? C28 C29 H29A 126.1 . . ? C30 C29 H29A 126.1 . . ? Fe2 C29 H29A 126.1 . . ? C31 C30 C29 108.6(3) . . ? C31 C30 Fe2 69.47(18) . . ? C29 C30 Fe2 69.88(18) . . ? C31 C30 H30A 125.7 . . ? C29 C30 H30A 125.7 . . ? Fe2 C30 H30A 125.7 . . ? C30 C31 C27 108.3(3) . . ? C30 C31 Fe2 70.07(18) . . ? C27 C31 Fe2 69.32(17) . . ? C30 C31 H31A 125.9 . . ? C27 C31 H31A 125.9 . . ? Fe2 C31 H31A 125.9 . . ? C36 C32 C33 107.8(3) . . ? C36 C32 Fe2 69.69(19) . . ? C33 C32 Fe2 69.3(2) . . ? C36 C32 H32A 126.1 . . ? C33 C32 H32A 126.1 . . ? Fe2 C32 H32A 126.1 . . ? C32 C33 C34 108.1(3) . . ? C32 C33 Fe2 70.13(19) . . ? C34 C33 Fe2 69.26(19) . . ? C32 C33 H33A 125.9 . . ? C34 C33 H33A 125.9 . . ? Fe2 C33 H33A 125.9 . . ? C35 C34 C33 107.8(3) . . ? C35 C34 Fe2 69.83(19) . . ? C33 C34 Fe2 69.85(19) . . ? C35 C34 H34A 126.1 . . ? C33 C34 H34A 126.1 . . ? Fe2 C34 H34A 126.1 . . ? C36 C35 C34 108.0(3) . . ? C36 C35 Fe2 70.1(2) . . ? C34 C35 Fe2 69.3(2) . . ? C36 C35 H35A 126.0 . . ? C34 C35 H35A 126.0 . . ? Fe2 C35 H35A 126.0 . . ? C35 C36 C32 108.3(3) . . ? C35 C36 Fe2 69.33(19) . . ? C32 C36 Fe2 69.82(19) . . ? C35 C36 H36A 125.9 . . ? C32 C36 H36A 125.9 . . ? Fe2 C36 H36A 125.9 . . ? C15 N1 N2 118.5(3) . . ? C15 N1 Ni1 127.2(2) . . ? N2 N1 Ni1 114.27(19) . . ? C1 N2 N1 107.5(2) . . ? C26 N3 N4 118.3(3) . . ? C26 N3 Ni1 127.5(2) . . ? N4 N3 Ni1 113.96(19) . . ? C8 N4 N3 107.2(2) . . ? C1 O1 Ni1 110.41(19) . . ? C8 O2 Ni1 110.58(19) . . ? Cl71 C70 Cl72 111.5(2) . . ? Cl71 C70 Cl73 110.1(2) . . ? Cl72 C70 Cl73 109.23(19) . . ? Cl71 C70 H70A 108.6 . . ? Cl72 C70 H70A 108.6 . . ? Cl73 C70 H70A 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 7.2(5) . . . . ? N2 C1 C2 C7 -172.9(3) . . . . ? O1 C1 C2 C3 -172.2(3) . . . . ? N2 C1 C2 C3 7.8(5) . . . . ? C7 C2 C3 C4 0.2(5) . . . . ? C1 C2 C3 C4 179.6(3) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? C3 C4 C5 C6 0.1(6) . . . . ? C4 C5 C6 C7 0.2(6) . . . . ? C5 C6 C7 C2 -0.3(5) . . . . ? C3 C2 C7 C6 0.1(5) . . . . ? C1 C2 C7 C6 -179.3(3) . . . . ? N4 C8 C9 C14 176.1(3) . . . . ? O2 C8 C9 C14 -4.6(4) . . . . ? N4 C8 C9 C10 -7.1(5) . . . . ? O2 C8 C9 C10 172.1(3) . . . . ? C14 C9 C10 C11 1.2(5) . . . . ? C8 C9 C10 C11 -175.6(3) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? C10 C11 C12 C13 -0.8(5) . . . . ? C11 C12 C13 C14 1.7(5) . . . . ? C12 C13 C14 C9 -1.1(5) . . . . ? C10 C9 C14 C13 -0.4(5) . . . . ? C8 C9 C14 C13 176.5(3) . . . . ? N1 C15 C16 C17 -179.8(3) . . . . ? N1 C15 C16 C20 -3.9(6) . . . . ? N1 C15 C16 Fe1 -94.9(4) . . . . ? C20 Fe1 C16 C17 -118.7(3) . . . . ? C22 Fe1 C16 C17 81.0(2) . . . . ? C21 Fe1 C16 C17 123.53(19) . . . . ? C23 Fe1 C16 C17 46.7(4) . . . . ? C24 Fe1 C16 C17 -160.3(4) . . . . ? C19 Fe1 C16 C17 -81.2(2) . . . . ? C25 Fe1 C16 C17 165.72(18) . . . . ? C18 Fe1 C16 C17 -37.21(18) . . . . ? C20 Fe1 C16 C15 126.6(3) . . . . ? C17 Fe1 C16 C15 -114.7(3) . . . . ? C22 Fe1 C16 C15 -33.7(3) . . . . ? C21 Fe1 C16 C15 8.8(3) . . . . ? C23 Fe1 C16 C15 -68.0(5) . . . . ? C24 Fe1 C16 C15 85.0(5) . . . . ? C19 Fe1 C16 C15 164.1(3) . . . . ? C25 Fe1 C16 C15 51.0(3) . . . . ? C18 Fe1 C16 C15 -151.9(3) . . . . ? C17 Fe1 C16 C20 118.7(3) . . . . ? C22 Fe1 C16 C20 -160.31(19) . . . . ? C21 Fe1 C16 C20 -117.81(19) . . . . ? C23 Fe1 C16 C20 165.3(3) . . . . ? C24 Fe1 C16 C20 -41.6(5) . . . . ? C19 Fe1 C16 C20 37.49(19) . . . . ? C25 Fe1 C16 C20 -75.6(2) . . . . ? C18 Fe1 C16 C20 81.4(2) . . . . ? C15 C16 C17 C18 177.7(3) . . . . ? C20 C16 C17 C18 0.9(4) . . . . ? Fe1 C16 C17 C18 59.9(2) . . . . ? C15 C16 C17 Fe1 117.9(3) . . . . ? C20 C16 C17 Fe1 -59.0(2) . . . . ? C20 Fe1 C17 C18 -81.0(2) . . . . ? C22 Fe1 C17 C18 121.9(2) . . . . ? C16 Fe1 C17 C18 -119.4(3) . . . . ? C21 Fe1 C17 C18 163.84(19) . . . . ? C23 Fe1 C17 C18 79.2(2) . . . . ? C24 Fe1 C17 C18 43.7(4) . . . . ? C19 Fe1 C17 C18 -37.6(2) . . . . ? C25 Fe1 C17 C18 -160.8(4) . . . . ? C20 Fe1 C17 C16 38.37(18) . . . . ? C22 Fe1 C17 C16 -118.73(19) . . . . ? C21 Fe1 C17 C16 -76.8(2) . . . . ? C23 Fe1 C17 C16 -161.38(18) . . . . ? C24 Fe1 C17 C16 163.0(3) . . . . ? C19 Fe1 C17 C16 81.8(2) . . . . ? C25 Fe1 C17 C16 -41.4(5) . . . . ? C18 Fe1 C17 C16 119.4(3) . . . . ? C16 C17 C18 C19 -0.6(4) . . . . ? Fe1 C17 C18 C19 58.7(2) . . . . ? C16 C17 C18 Fe1 -59.3(2) . . . . ? C20 Fe1 C18 C17 82.7(2) . . . . ? C22 Fe1 C18 C17 -77.8(2) . . . . ? C16 Fe1 C18 C17 38.07(19) . . . . ? C21 Fe1 C18 C17 -45.9(5) . . . . ? C23 Fe1 C18 C17 -119.1(2) . . . . ? C24 Fe1 C18 C17 -161.44(19) . . . . ? C19 Fe1 C18 C17 119.8(3) . . . . ? C25 Fe1 C18 C17 165.5(3) . . . . ? C20 Fe1 C18 C19 -37.1(2) . . . . ? C17 Fe1 C18 C19 -119.8(3) . . . . ? C22 Fe1 C18 C19 162.5(2) . . . . ? C16 Fe1 C18 C19 -81.7(2) . . . . ? C21 Fe1 C18 C19 -165.7(4) . . . . ? C23 Fe1 C18 C19 121.2(2) . . . . ? C24 Fe1 C18 C19 78.8(2) . . . . ? C25 Fe1 C18 C19 45.7(4) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? Fe1 C18 C19 C20 58.8(2) . . . . ? C17 C18 C19 Fe1 -58.7(2) . . . . ? C17 Fe1 C19 C20 -82.8(2) . . . . ? C22 Fe1 C19 C20 -168.0(4) . . . . ? C16 Fe1 C19 C20 -38.40(19) . . . . ? C21 Fe1 C19 C20 48.8(4) . . . . ? C23 Fe1 C19 C20 162.23(19) . . . . ? C24 Fe1 C19 C20 121.2(2) . . . . ? C25 Fe1 C19 C20 79.7(2) . . . . ? C18 Fe1 C19 C20 -120.0(3) . . . . ? C20 Fe1 C19 C18 120.0(3) . . . . ? C17 Fe1 C19 C18 37.11(19) . . . . ? C22 Fe1 C19 C18 -48.0(5) . . . . ? C16 Fe1 C19 C18 81.6(2) . . . . ? C21 Fe1 C19 C18 168.7(3) . . . . ? C23 Fe1 C19 C18 -77.8(2) . . . . ? C24 Fe1 C19 C18 -118.9(2) . . . . ? C25 Fe1 C19 C18 -160.3(2) . . . . ? C18 C19 C20 C16 0.4(4) . . . . ? Fe1 C19 C20 C16 59.5(2) . . . . ? C18 C19 C20 Fe1 -59.1(2) . . . . ? C17 C16 C20 C19 -0.8(4) . . . . ? C15 C16 C20 C19 -177.2(3) . . . . ? Fe1 C16 C20 C19 -59.9(2) . . . . ? C17 C16 C20 Fe1 59.1(2) . . . . ? C15 C16 C20 Fe1 -117.3(4) . . . . ? C17 Fe1 C20 C19 80.7(2) . . . . ? C22 Fe1 C20 C19 169.2(3) . . . . ? C16 Fe1 C20 C19 119.0(3) . . . . ? C21 Fe1 C20 C19 -159.4(2) . . . . ? C23 Fe1 C20 C19 -45.7(5) . . . . ? C24 Fe1 C20 C19 -76.6(2) . . . . ? C25 Fe1 C20 C19 -117.7(2) . . . . ? C18 Fe1 C20 C19 37.5(2) . . . . ? C17 Fe1 C20 C16 -38.21(19) . . . . ? C22 Fe1 C20 C16 50.2(4) . . . . ? C21 Fe1 C20 C16 81.6(2) . . . . ? C23 Fe1 C20 C16 -164.6(3) . . . . ? C24 Fe1 C20 C16 164.41(19) . . . . ? C19 Fe1 C20 C16 -119.0(3) . . . . ? C25 Fe1 C20 C16 123.33(19) . . . . ? C18 Fe1 C20 C16 -81.5(2) . . . . ? C20 Fe1 C21 C22 -162.8(2) . . . . ? C17 Fe1 C21 C22 -76.7(2) . . . . ? C16 Fe1 C21 C22 -119.2(2) . . . . ? C23 Fe1 C21 C22 37.8(2) . . . . ? C24 Fe1 C21 C22 81.7(2) . . . . ? C19 Fe1 C21 C22 162.1(3) . . . . ? C25 Fe1 C21 C22 119.2(3) . . . . ? C18 Fe1 C21 C22 -41.8(5) . . . . ? C20 Fe1 C21 C25 78.0(2) . . . . ? C17 Fe1 C21 C25 164.1(2) . . . . ? C22 Fe1 C21 C25 -119.2(3) . . . . ? C16 Fe1 C21 C25 121.6(2) . . . . ? C23 Fe1 C21 C25 -81.4(2) . . . . ? C24 Fe1 C21 C25 -37.5(2) . . . . ? C19 Fe1 C21 C25 42.9(4) . . . . ? C18 Fe1 C21 C25 -161.0(4) . . . . ? C25 C21 C22 C23 -0.1(4) . . . . ? Fe1 C21 C22 C23 -59.7(2) . . . . ? C25 C21 C22 Fe1 59.6(2) . . . . ? C20 Fe1 C22 C23 161.7(3) . . . . ? C17 Fe1 C22 C23 -117.7(2) . . . . ? C16 Fe1 C22 C23 -161.11(19) . . . . ? C21 Fe1 C22 C23 118.9(3) . . . . ? C24 Fe1 C22 C23 37.7(2) . . . . ? C19 Fe1 C22 C23 -39.7(5) . . . . ? C25 Fe1 C22 C23 81.2(2) . . . . ? C18 Fe1 C22 C23 -75.9(2) . . . . ? C20 Fe1 C22 C21 42.8(4) . . . . ? C17 Fe1 C22 C21 123.4(2) . . . . ? C16 Fe1 C22 C21 80.0(2) . . . . ? C23 Fe1 C22 C21 -118.9(3) . . . . ? C24 Fe1 C22 C21 -81.2(2) . . . . ? C19 Fe1 C22 C21 -158.6(4) . . . . ? C25 Fe1 C22 C21 -37.7(2) . . . . ? C18 Fe1 C22 C21 165.2(2) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? Fe1 C22 C23 C24 -59.4(2) . . . . ? C21 C22 C23 Fe1 59.6(2) . . . . ? C20 Fe1 C23 C22 -161.1(3) . . . . ? C17 Fe1 C23 C22 81.4(2) . . . . ? C16 Fe1 C23 C22 47.0(4) . . . . ? C21 Fe1 C23 C22 -37.9(2) . . . . ? C24 Fe1 C23 C22 -119.3(3) . . . . ? C19 Fe1 C23 C22 165.2(2) . . . . ? C25 Fe1 C23 C22 -81.9(2) . . . . ? C18 Fe1 C23 C22 123.2(2) . . . . ? C20 Fe1 C23 C24 -41.8(5) . . . . ? C17 Fe1 C23 C24 -159.3(2) . . . . ? C22 Fe1 C23 C24 119.3(3) . . . . ? C16 Fe1 C23 C24 166.2(3) . . . . ? C21 Fe1 C23 C24 81.4(2) . . . . ? C19 Fe1 C23 C24 -75.5(2) . . . . ? C25 Fe1 C23 C24 37.4(2) . . . . ? C18 Fe1 C23 C24 -117.6(2) . . . . ? C22 C23 C24 C25 -0.3(4) . . . . ? Fe1 C23 C24 C25 -59.7(2) . . . . ? C22 C23 C24 Fe1 59.4(2) . . . . ? C20 Fe1 C24 C25 -77.0(2) . . . . ? C17 Fe1 C24 C25 168.6(3) . . . . ? C22 Fe1 C24 C25 81.8(2) . . . . ? C16 Fe1 C24 C25 -45.6(5) . . . . ? C21 Fe1 C24 C25 37.85(19) . . . . ? C23 Fe1 C24 C25 119.3(3) . . . . ? C19 Fe1 C24 C25 -118.1(2) . . . . ? C18 Fe1 C24 C25 -159.98(19) . . . . ? C20 Fe1 C24 C23 163.7(2) . . . . ? C17 Fe1 C24 C23 49.3(4) . . . . ? C22 Fe1 C24 C23 -37.6(2) . . . . ? C16 Fe1 C24 C23 -165.0(3) . . . . ? C21 Fe1 C24 C23 -81.5(2) . . . . ? C19 Fe1 C24 C23 122.6(2) . . . . ? C25 Fe1 C24 C23 -119.3(3) . . . . ? C18 Fe1 C24 C23 80.7(2) . . . . ? C23 C24 C25 C21 0.2(4) . . . . ? Fe1 C24 C25 C21 -59.1(2) . . . . ? C23 C24 C25 Fe1 59.4(2) . . . . ? C22 C21 C25 C24 -0.1(4) . . . . ? Fe1 C21 C25 C24 59.3(2) . . . . ? C22 C21 C25 Fe1 -59.4(2) . . . . ? C20 Fe1 C25 C24 120.9(2) . . . . ? C17 Fe1 C25 C24 -165.4(4) . . . . ? C22 Fe1 C25 C24 -81.4(2) . . . . ? C16 Fe1 C25 C24 162.82(19) . . . . ? C21 Fe1 C25 C24 -119.1(3) . . . . ? C23 Fe1 C25 C24 -37.7(2) . . . . ? C19 Fe1 C25 C24 79.2(2) . . . . ? C18 Fe1 C25 C24 46.3(4) . . . . ? C20 Fe1 C25 C21 -120.0(2) . . . . ? C17 Fe1 C25 C21 -46.2(5) . . . . ? C22 Fe1 C25 C21 37.7(2) . . . . ? C16 Fe1 C25 C21 -78.1(2) . . . . ? C23 Fe1 C25 C21 81.4(2) . . . . ? C24 Fe1 C25 C21 119.1(3) . . . . ? C19 Fe1 C25 C21 -161.7(2) . . . . ? C18 Fe1 C25 C21 165.4(3) . . . . ? N3 C26 C27 C31 -2.1(6) . . . . ? N3 C26 C27 C28 -176.7(3) . . . . ? N3 C26 C27 Fe2 -91.8(4) . . . . ? C34 Fe2 C27 C31 -83.6(2) . . . . ? C35 Fe2 C27 C31 -126.76(19) . . . . ? C28 Fe2 C27 C31 118.4(3) . . . . ? C33 Fe2 C27 C31 -49.3(4) . . . . ? C30 Fe2 C27 C31 37.25(19) . . . . ? C36 Fe2 C27 C31 -166.7(2) . . . . ? C32 Fe2 C27 C31 163.1(6) . . . . ? C29 Fe2 C27 C31 81.1(2) . . . . ? C34 Fe2 C27 C28 158.08(19) . . . . ? C35 Fe2 C27 C28 114.9(2) . . . . ? C31 Fe2 C27 C28 -118.4(3) . . . . ? C33 Fe2 C27 C28 -167.6(3) . . . . ? C30 Fe2 C27 C28 -81.1(2) . . . . ? C36 Fe2 C27 C28 74.9(2) . . . . ? C32 Fe2 C27 C28 44.7(7) . . . . ? C29 Fe2 C27 C28 -37.22(19) . . . . ? C34 Fe2 C27 C26 41.8(3) . . . . ? C35 Fe2 C27 C26 -1.4(3) . . . . ? C28 Fe2 C27 C26 -116.3(3) . . . . ? C31 Fe2 C27 C26 125.4(3) . . . . ? C33 Fe2 C27 C26 76.1(4) . . . . ? C30 Fe2 C27 C26 162.6(3) . . . . ? C36 Fe2 C27 C26 -41.4(3) . . . . ? C32 Fe2 C27 C26 -71.5(7) . . . . ? C29 Fe2 C27 C26 -153.5(3) . . . . ? C31 C27 C28 C29 0.2(4) . . . . ? C26 C27 C28 C29 175.9(3) . . . . ? Fe2 C27 C28 C29 59.6(2) . . . . ? C31 C27 C28 Fe2 -59.5(2) . . . . ? C26 C27 C28 Fe2 116.2(3) . . . . ? C34 Fe2 C28 C29 -165.9(3) . . . . ? C27 Fe2 C28 C29 -119.6(3) . . . . ? C35 Fe2 C28 C29 156.97(19) . . . . ? C31 Fe2 C28 C29 -81.2(2) . . . . ? C33 Fe2 C28 C29 35.3(6) . . . . ? C30 Fe2 C28 C29 -37.69(19) . . . . ? C36 Fe2 C28 C29 113.5(2) . . . . ? C32 Fe2 C28 C29 72.1(2) . . . . ? C34 Fe2 C28 C27 -46.3(4) . . . . ? C35 Fe2 C28 C27 -83.4(2) . . . . ? C31 Fe2 C28 C27 38.40(18) . . . . ? C33 Fe2 C28 C27 155.0(5) . . . . ? C30 Fe2 C28 C27 81.9(2) . . . . ? C36 Fe2 C28 C27 -126.9(2) . . . . ? C32 Fe2 C28 C27 -168.28(19) . . . . ? C29 Fe2 C28 C27 119.6(3) . . . . ? C27 C28 C29 C30 -0.2(4) . . . . ? Fe2 C28 C29 C30 58.7(2) . . . . ? C27 C28 C29 Fe2 -59.0(2) . . . . ? C34 Fe2 C29 C28 154.9(5) . . . . ? C27 Fe2 C29 C28 37.99(19) . . . . ? C35 Fe2 C29 C28 -49.7(4) . . . . ? C31 Fe2 C29 C28 82.4(2) . . . . ? C33 Fe2 C29 C28 -169.7(2) . . . . ? C30 Fe2 C29 C28 119.5(3) . . . . ? C36 Fe2 C29 C28 -85.5(2) . . . . ? C32 Fe2 C29 C28 -128.4(2) . . . . ? C34 Fe2 C29 C30 35.4(6) . . . . ? C27 Fe2 C29 C30 -81.51(19) . . . . ? C35 Fe2 C29 C30 -169.2(3) . . . . ? C28 Fe2 C29 C30 -119.5(3) . . . . ? C31 Fe2 C29 C30 -37.13(18) . . . . ? C33 Fe2 C29 C30 70.8(2) . . . . ? C36 Fe2 C29 C30 155.05(19) . . . . ? C32 Fe2 C29 C30 112.1(2) . . . . ? C28 C29 C30 C31 0.2(4) . . . . ? Fe2 C29 C30 C31 58.9(2) . . . . ? C28 C29 C30 Fe2 -58.6(2) . . . . ? C34 Fe2 C30 C31 70.9(2) . . . . ? C27 Fe2 C30 C31 -37.95(18) . . . . ? C35 Fe2 C30 C31 41.8(6) . . . . ? C28 Fe2 C30 C31 -82.5(2) . . . . ? C33 Fe2 C30 C31 111.7(2) . . . . ? C36 Fe2 C30 C31 -173.6(3) . . . . ? C32 Fe2 C30 C31 154.03(19) . . . . ? C29 Fe2 C30 C31 -120.0(3) . . . . ? C34 Fe2 C30 C29 -169.10(19) . . . . ? C27 Fe2 C30 C29 82.01(19) . . . . ? C35 Fe2 C30 C29 161.8(4) . . . . ? C28 Fe2 C30 C29 37.43(18) . . . . ? C31 Fe2 C30 C29 120.0(3) . . . . ? C33 Fe2 C30 C29 -128.4(2) . . . . ? C36 Fe2 C30 C29 -53.6(4) . . . . ? C32 Fe2 C30 C29 -86.0(2) . . . . ? C29 C30 C31 C27 -0.1(4) . . . . ? Fe2 C30 C31 C27 59.0(2) . . . . ? C29 C30 C31 Fe2 -59.1(2) . . . . ? C28 C27 C31 C30 0.0(4) . . . . ? C26 C27 C31 C30 -175.3(3) . . . . ? Fe2 C27 C31 C30 -59.4(2) . . . . ? C28 C27 C31 Fe2 59.4(2) . . . . ? C26 C27 C31 Fe2 -115.8(3) . . . . ? C34 Fe2 C31 C30 -127.4(2) . . . . ? C27 Fe2 C31 C30 119.6(3) . . . . ? C35 Fe2 C31 C30 -167.09(19) . . . . ? C28 Fe2 C31 C30 81.0(2) . . . . ? C33 Fe2 C31 C30 -84.7(2) . . . . ? C36 Fe2 C31 C30 167.8(5) . . . . ? C32 Fe2 C31 C30 -52.7(4) . . . . ? C29 Fe2 C31 C30 37.45(19) . . . . ? C34 Fe2 C31 C27 113.1(2) . . . . ? C35 Fe2 C31 C27 73.3(2) . . . . ? C28 Fe2 C31 C27 -38.52(19) . . . . ? C33 Fe2 C31 C27 155.70(19) . . . . ? C30 Fe2 C31 C27 -119.6(3) . . . . ? C36 Fe2 C31 C27 48.3(6) . . . . ? C32 Fe2 C31 C27 -172.2(3) . . . . ? C29 Fe2 C31 C27 -82.1(2) . . . . ? C34 Fe2 C32 C36 -81.5(2) . . . . ? C27 Fe2 C32 C36 37.2(7) . . . . ? C35 Fe2 C32 C36 -37.4(2) . . . . ? C28 Fe2 C32 C36 73.8(3) . . . . ? C31 Fe2 C32 C36 -166.1(3) . . . . ? C33 Fe2 C32 C36 -119.3(3) . . . . ? C30 Fe2 C32 C36 158.0(2) . . . . ? C29 Fe2 C32 C36 114.5(2) . . . . ? C34 Fe2 C32 C33 37.8(2) . . . . ? C27 Fe2 C32 C33 156.5(6) . . . . ? C35 Fe2 C32 C33 81.9(2) . . . . ? C28 Fe2 C32 C33 -166.9(2) . . . . ? C31 Fe2 C32 C33 -46.8(4) . . . . ? C30 Fe2 C32 C33 -82.7(2) . . . . ? C36 Fe2 C32 C33 119.3(3) . . . . ? C29 Fe2 C32 C33 -126.2(2) . . . . ? C36 C32 C33 C34 0.2(4) . . . . ? Fe2 C32 C33 C34 -59.0(2) . . . . ? C36 C32 C33 Fe2 59.3(2) . . . . ? C34 Fe2 C33 C32 -119.4(3) . . . . ? C27 Fe2 C33 C32 -169.3(3) . . . . ? C35 Fe2 C33 C32 -81.4(2) . . . . ? C28 Fe2 C33 C32 45.9(6) . . . . ? C31 Fe2 C33 C32 156.7(2) . . . . ? C30 Fe2 C33 C32 114.3(2) . . . . ? C36 Fe2 C33 C32 -37.6(2) . . . . ? C29 Fe2 C33 C32 74.1(3) . . . . ? C27 Fe2 C33 C34 -50.0(4) . . . . ? C35 Fe2 C33 C34 38.0(2) . . . . ? C28 Fe2 C33 C34 165.2(5) . . . . ? C31 Fe2 C33 C34 -84.0(2) . . . . ? C30 Fe2 C33 C34 -126.4(2) . . . . ? C36 Fe2 C33 C34 81.8(2) . . . . ? C32 Fe2 C33 C34 119.4(3) . . . . ? C29 Fe2 C33 C34 -166.5(2) . . . . ? C32 C33 C34 C35 -0.2(4) . . . . ? Fe2 C33 C34 C35 -59.8(2) . . . . ? C32 C33 C34 Fe2 59.6(2) . . . . ? C27 Fe2 C34 C35 -85.9(2) . . . . ? C28 Fe2 C34 C35 -53.4(4) . . . . ? C31 Fe2 C34 C35 -128.9(2) . . . . ? C33 Fe2 C34 C35 118.8(3) . . . . ? C30 Fe2 C34 C35 -168.55(19) . . . . ? C36 Fe2 C34 C35 37.6(2) . . . . ? C32 Fe2 C34 C35 81.3(2) . . . . ? C29 Fe2 C34 C35 163.5(5) . . . . ? C27 Fe2 C34 C33 155.3(2) . . . . ? C35 Fe2 C34 C33 -118.8(3) . . . . ? C28 Fe2 C34 C33 -172.2(3) . . . . ? C31 Fe2 C34 C33 112.3(2) . . . . ? C30 Fe2 C34 C33 72.6(3) . . . . ? C36 Fe2 C34 C33 -81.2(2) . . . . ? C32 Fe2 C34 C33 -37.5(2) . . . . ? C29 Fe2 C34 C33 44.6(6) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? Fe2 C34 C35 C36 -59.7(2) . . . . ? C33 C34 C35 Fe2 59.8(2) . . . . ? C34 Fe2 C35 C36 119.2(3) . . . . ? C27 Fe2 C35 C36 -129.47(19) . . . . ? C28 Fe2 C35 C36 -85.9(2) . . . . ? C31 Fe2 C35 C36 -170.99(19) . . . . ? C33 Fe2 C35 C36 81.1(2) . . . . ? C30 Fe2 C35 C36 156.1(4) . . . . ? C32 Fe2 C35 C36 37.4(2) . . . . ? C29 Fe2 C35 C36 -51.1(4) . . . . ? C27 Fe2 C35 C34 111.4(2) . . . . ? C28 Fe2 C35 C34 154.9(2) . . . . ? C31 Fe2 C35 C34 69.8(2) . . . . ? C33 Fe2 C35 C34 -38.0(2) . . . . ? C30 Fe2 C35 C34 36.9(6) . . . . ? C36 Fe2 C35 C34 -119.2(3) . . . . ? C32 Fe2 C35 C34 -81.8(2) . . . . ? C29 Fe2 C35 C34 -170.3(3) . . . . ? C34 C35 C36 C32 0.1(4) . . . . ? Fe2 C35 C36 C32 -59.2(2) . . . . ? C34 C35 C36 Fe2 59.2(2) . . . . ? C33 C32 C36 C35 -0.2(4) . . . . ? Fe2 C32 C36 C35 58.8(2) . . . . ? C33 C32 C36 Fe2 -59.0(2) . . . . ? C34 Fe2 C36 C35 -37.9(2) . . . . ? C27 Fe2 C36 C35 70.3(2) . . . . ? C28 Fe2 C36 C35 113.0(2) . . . . ? C31 Fe2 C36 C35 31.3(6) . . . . ? C33 Fe2 C36 C35 -82.0(2) . . . . ? C30 Fe2 C36 C35 -166.2(3) . . . . ? C32 Fe2 C36 C35 -119.7(3) . . . . ? C29 Fe2 C36 C35 156.38(19) . . . . ? C34 Fe2 C36 C32 81.8(2) . . . . ? C27 Fe2 C36 C32 -170.0(2) . . . . ? C35 Fe2 C36 C32 119.7(3) . . . . ? C28 Fe2 C36 C32 -127.3(2) . . . . ? C31 Fe2 C36 C32 151.0(5) . . . . ? C33 Fe2 C36 C32 37.7(2) . . . . ? C30 Fe2 C36 C32 -46.5(4) . . . . ? C29 Fe2 C36 C32 -83.9(2) . . . . ? C16 C15 N1 N2 2.1(5) . . . . ? C16 C15 N1 Ni1 -177.5(3) . . . . ? O2 Ni1 N1 C15 2.2(3) . . . . ? O1 Ni1 N1 C15 -175.9(3) . . . . ? N3 Ni1 N1 C15 77.5(17) . . . . ? O2 Ni1 N1 N2 -177.4(2) . . . . ? O1 Ni1 N1 N2 4.5(2) . . . . ? N3 Ni1 N1 N2 -102.1(16) . . . . ? O1 C1 N2 N1 1.1(4) . . . . ? C2 C1 N2 N1 -178.8(3) . . . . ? C15 N1 N2 C1 176.2(3) . . . . ? Ni1 N1 N2 C1 -4.2(3) . . . . ? C27 C26 N3 N4 0.9(5) . . . . ? C27 C26 N3 Ni1 -173.5(2) . . . . ? O2 Ni1 N3 C26 173.3(3) . . . . ? O1 Ni1 N3 C26 -8.5(3) . . . . ? N1 Ni1 N3 C26 97.6(17) . . . . ? O2 Ni1 N3 N4 -1.31(19) . . . . ? O1 Ni1 N3 N4 176.86(19) . . . . ? N1 Ni1 N3 N4 -77.0(17) . . . . ? O2 C8 N4 N3 -0.3(4) . . . . ? C9 C8 N4 N3 178.9(2) . . . . ? C26 N3 N4 C8 -174.0(3) . . . . ? Ni1 N3 N4 C8 1.2(3) . . . . ? N2 C1 O1 Ni1 2.4(4) . . . . ? C2 C1 O1 Ni1 -177.6(2) . . . . ? O2 Ni1 O1 C1 -59(2) . . . . ? N1 Ni1 O1 C1 -3.7(2) . . . . ? N3 Ni1 O1 C1 172.6(2) . . . . ? N4 C8 O2 Ni1 -0.7(4) . . . . ? C9 C8 O2 Ni1 -180.0(2) . . . . ? O1 Ni1 O2 C8 -128(2) . . . . ? N1 Ni1 O2 C8 177.4(2) . . . . ? N3 Ni1 O2 C8 1.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.516 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.083